Category: 627-31-6

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), A new synthetic method of this compound is introduced below., COA of Formula: C3H6I2

Preparation of 1,3-bis(1-isoquinolyl)-propane 2a; A solution of 2-benzoyl-1-cyano-1,2-dihydroisoquinoline 1a (5.0 g; 19.2 mmol) and of 1,3-diiodopropane (1.1 mL; 9.6 mmol) in DMF (15 mL) was dropwise added to a stirred suspension of sodium hydride (0.46 g; 19.2 mmol) in DMF (30 mL) at -10 C. The content was stirred for 4 h and poured into ice-cold water (200 mL). The creamy solid was filtered off. After drying, the solid was hydrolyzed by treatment with 50% aqueous NaOH in EtOH at reflux. After removal of EtOH, the crude residue was dissolved in ArMe (50 mL) and water (50 mL). The organic layer was collected, washed with water (50 mL) and then extracted with 1N aqueous HCl (2×50 mL). The acidic layers were basified with concentrated NH4OH and finally extracted with CH2Cl2 (3×30 mL). The organic layers were dried over anhydrous MgSO4 and evaporated under reduced pressure to afford a white solid which recrystallized from petroleum ether 100-140 (2.5 g); yield, 40%; mp 96-97 C.1H-NMR (CDCl3) delta 2.49 (pentuplet, 2H, J=7.7 Hz), 3.50 (t, 4H, J=7.7 Hz), 7.51 (d, 2H, J=5.7 Hz), 7.56 (t, 2H, J=7.5 Hz), 7.65 (t, 2H, J=7.5 Hz), 7.80 (d, 2H, J=7.5 Hz), 8.18 (d, 2H, J=7.5 Hz), 8.44 (d, 2H, J=5.7 Hz)Anal. C21H18N2 (298.389) Calc. N, 9.39; C, 84.53; H, 6.08. Found N, 9.56; C, 84.38; H, 6.16.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 627-31-6 as follows. Quality Control of 1,3-Diiodopropane(stabilized with Copper chip)

The beta- lactam carbonyl compound shown in the formula CH3CH2-COCH2CONH-C6H4Cl1.0mmol added 50 ml round-bottomed flask, and then sequentially adding K2CO32.4mmol, 0.10 mmol tetrabutylammonium chloride, ammonium acetate 1.1mmol, 1,3Diiodopropane 1.2mmol and 35mL of deionized water and mix well. The reaction was continued stirring at 20 10.0 hours, the reaction was stopped by filtration, dried and purified by recrystallization after give 6- (4-chloro-anilino) -5-propionyl-3,4-dihydropyran, products yield 96%.

According to the analysis of related databases, 627-31-6, the application of this compound in the production field has become more and more popular.

These common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 1,3-Diiodopropane(stabilized with Copper chip)

Examples 13 -22; Synthesis of PBD dimers linked at the C-8 position; n=3, 4,5, 6, 7, 8,9, 10, 11, 12 Example 13 (n=3); (a) 1,1′-[(Propane-1,3-diyl)dioxy]bis[(11S,11aS)-10-(tert- butyloxycarbonyl)-7-methoxy-l1- (tetrahydro-pyran-2-yloxy)- 1,2, 3, 10, 11, IIa-hexahydro-5H-pyrrolo (2, 1-cJ [l, 4] benzodiazepine-5- one] (15a); 1,3-Diiodopropane (66 mg, 0.22 mmol, 0.5 equiv) was added to the mixture of monomer 14 (0.2 g, 0.44 mmol, 1. 0 equiv) and potassium carbonate (0. 98mmol, 2.2 equiv) in dry DMF (30 mL), and the resulting mixture was heated to 90C under a nitrogen atmosphere for 5 h. Removal of excess solvent under reduced pressure afforded a crude solid, which was subjected to flash column chromatography (SiO2, 50% EtOAc-hexane) to afford the dimerized compound 15a (90 mg, 0.09 mmol, 43% yield, mixture of diastereomers from THP protecting group) as a solid: [a] 20D = +57 (c = 0.14, CHCl3); 1H NMR (CDC13, 400 MHz): 5 1. 20-1. 84 (m, 60H, Boc, THP), 1.91-2. 20 (m, 16H, 1-H, 2-H), 2.34-2. 46 (m, 4H, 13-H), 3.40-3. 74 (m, 16H, 3-H, lla-H, THP), 3.79-3. 99 (m, 16H, 7-OMe, THP), 4.12-4. 30 (m, 8H, 12- H), 4.97-5. 15 (m, 4H, THP), 5.66-5. 75 (d, 2H, 11-H), 5. 77-5.89 (d, 2H, 11-H), 6.55 (s, 2H, 9-H), 6.89 (s, 2H, 9-H), 7.16 (s, 2H, 6- H), 7.20 (s, 2H, 6-H) ; 13C NMR (CDCl3, 400 MHz): 6 19.9, 20.5, 23. 1,23. 2,25. 2,25. 3,28. 1,28. 2,28. 9,29. 0, 29. 1,30. 9,31. 3, 46.3, 56.0, 56.1, 60.0, 60.2, 63.4, 64.5, 65.3, 65.7, 81.0, 81.1, 88. 1,91. 2,95. 7,100. 3,110. 1,110. 8, 114.7, 115.2, 127.5, 129.8, 148.5, 148. 8, 150.0, 155.1, 167.4, 167.6 ; IR (neat): 3426, 2943, 1703, 1643,1604, 1513, 1454,1432, 1326,1270, 1201,1163, 1023cm~ r MS (FAB) m/z (relative intensity) 959 ([M + Na]+., 100), 937 (M 62), 835 (67), 735 (60).

The synthetic route of 1,3-Diiodopropane(stabilized with Copper chip) has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 627-31-6, COA of Formula: C3H6I2

In a 25 mL flask, xanthene (1, 350 mg, 1.92 mmol),dissolved in dry THF (10 mL) and diiodopropane (0.2 mL 1.74 mmol) were stirred under argon at 0 C. n-Butyllithium (1 mL, solution 2.5 M in hexanes) was added dropwise, after which the reactionwas heated up to room temperature. After approx 2 h (TLC 40% hexane-CHCl3 7:3), solvent was evaporated in vacuo. The crude product was dissolved in DCM (75 mL), washed three times withwater (30 mL), dried over Na2SO4 and taken to dryness in vacuo. The crude product was purified byflash column chromatography (0%-40% CHCl3 in hexane), to give 12 as a white powder, (410 mg,0.93 mmol, 48% yield).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Related Products of 627-31-6,Some common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), molecular formula is C3H6I2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

3,5-bis(4-iodobutyl) pyridine was prepared following a modifiedprocedure reported in the literature [24,25]. 3,5-dimethyl pyridine(1.5 g, 16.0 mmol) in dry THF (32 mL) was treated with Lithium diisopropylamide(19.3 mmol) under nitrogen atmosphere at -30 C for1 h. 1,3-diiodopropane (7.8 g, 32.2 mmol) was then added quickly intothe reaction mixture to produce 3,5-bis(4-bromobutyl)pyridine. Theproduct was purified by silica gel column chromatography using amixture of hexane/EA as eluent to get a light brown colour oil compound(2). Here the yield is around 82%. The synthesis of compound(3) 3,5-bis(4-bromobutyl)pyridine has been done by the same procedureas of compound (2). The synthetic route is given in Scheme 2. 2.2.1.1. Compound 2. 1H NMR (400 MHz, DMSO-d6): delta(ppm) 8.11 (s,2H), 7.59 (s, 1H), 3.33 (t, 4H), 2.67 (t, 4H), 1.82 (m, 4H), 1.59 (m, 4H),13C NMR (100 MHz, CDCl3): delta(ppm) 147.3, 139.7, 137.1, 32.6, 30.1,28.6, 27.3.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Diiodopropane(stabilized with Copper chip), its application will become more common.

Reference:
Retracted Article; Vekariya, Rohit L.; Dhar, Abhishek; Kumar, Nadavala Siva; Pal, Rumpa; Roy, Subhasis; Organic electronics; vol. 51; (2017); p. 477 – 484;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 627-31-6, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 627-31-6 name is 1,3-Diiodopropane(stabilized with Copper chip), This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: K2CO3 (3.7g, 26.8mmol) was added to a solution of 3-(4-hydroxyphenyl)-thiazolidine-2,4-dione (10, 2.8g, 13.4mmol) in MeCN (20mL) and stirred for 10min. The appropriate diiodoalkane (80.3mmol) was added and the reaction mixture was stirred at 95C for 7h. After cooling, water (10mL) was added followed by extraction with ethyl acetate. The organic layer was dried over anhydrous MgSO4, filtered and evaporated under reduced pressure. The residue was purified by flash column chromatography (SiO2, n-hexane/ethyl acetate= 3/1 v/v) to afford the desired compounds.4.1.5 61 3-(4-(3-Iodopropoxy)phenyl)thiazolidine-2,4-dione (11a) (0021) White solid, yield: 81%, 4.0g, 1H NMR (400MHz, DMSO-d6) delta: 2.19-2.24 (m, 2H), 3.39 (t, J=6.6Hz, 2H), 4.06 (t, J=4.7Hz, 2H), 4.28 (s, 2H), 7.05 (d, J=7.1Hz, 2H), 7.20 (d, J=7.1Hz, 2H). HRMS (ES+): m/z calculated for C12H12INO3S: 399.9481 [M+Na]+. Found 399.9472.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

These common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. COA of Formula: C3H6I2

Nitrogen-extractedIn a 250 ml three-necked bottle, 2.33 g (1H-indol-2-yl)-1H-benzo[d]imidazole was weighed.(10 mmol), add 50 ml of dimethylformamide, stir well.Then add 2.8 g of potassium hydroxide (50 mmol) and stir at room temperature for 2-36 hours.As most of the potassium hydroxide dissolves, a thick, cloudy solution forms.Add 1.72 ml of 1,3-diiodopropane (15 mmol) and react at room temperature for 18-24 hours. Point board monitoring,When the reaction of raw materials is complete,The reaction was stopped and 40 ml of water and 30 ml of dichloromethane were added to the system.The mixture was further extracted with 30 ml of dichloromethane three times and the organic phases were combined and dried over anhydrous magnesium sulfate.After concentrating the organic phasePurification by column chromatography7,8-Dihydro-6H-benzo[4′,5′]imidazo[2′,1′:3,4][1,4]diaza [1,2-a]fluorene Body 1.23g, yield 45%, can be directly put into the next step reaction.

The synthetic route of 1,3-Diiodopropane(stabilized with Copper chip) has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hong Kong University Of Science And Technology Shenzhen Institute; Kuang Fuer; Li Dongsheng; Cai Peiying; (20 pag.)CN107459533; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

To a solution of ethyl 2-(6-nitropyridin-3-yl)acetate (33.0 g, 157 mmol) in DMF (150 mL) was added NaH (13.2 g, 330 mmol) (60 % in oil) at 0 C. The reaction mixture was allowed to warm to RT and stirred for 15 min. The mixture was cooled to 0 C again before 1,3- diiodopropane (37.3 mL, 325 mmol) was added. The resulting mixture was stirred at 0 C for 30 min, then warmed to RT and stirred for 1 h. The mixture was quenched with sat. NH4C1 (500 mL), diluted with water (500 mL), then extracted with EtOAc (500 mLx3). The combined organic layers were washed with brine (200 mL), dried over Na2SC>4, filtered, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (Petroleum ether/ EtOAc =30/ 1 to 20/ 1) to give the title compound. MS (EI) m/z 251 [M+H]+.

The synthetic route of 627-31-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ZHOU, Hua; FRADERA, Xavier; HAN, Yongxin; MCGOWAN, Meredeth, A.; SCIAMMETTA, Nunzio; WHITE, Catherine; YU, Wensheng; (89 pag.)WO2019/27856; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C3H6I2

Example 39 l-(2-[(2,6-difluorophenyl)methoxyl-l,l,l,3,3,3-hexafluoropropan-2-yl|-4-[l-(4- fluorobenzenesulfonyl)cyclobutyl”|benzene Sodium hydride (14.75 mg, 0.369 mmol, 60%> suspension in mineral oil) was added to a solution of l,3-difluoro-2-(((l,l,l,3,3,3-hexafluoro-2-(4-(((4- fluorophenyl)sulfonyl)methyl)phenyl)propan-2-yl)oxy)methyl)benzene (20 mg, 0.037 mmol) and 1,3-diiodopropane (10.91 mg, 0.037 mmol) in Nu,Nu-dimethylformamide (1 mL). After 1 h at room temperature, saturated ammonium chloride (2 mL) and ethyl acetate (15 mL) were added. The mixture was washed with water (2×5 mL), brine (5 mL), dried (magnesium sulfate), filtered and concentrated under reduced pressure. The crude material was purified via preparative LC/MS with the following conditions: Column: Waters XBridge CI 8, 19 x 150 mm, 5-muiotaeta particles; Mobile Phase A: 5:95 acetonitrile: water with 10-mM ammonium acetate; Mobile Phase B: 95:5 acetonitrile: water with 10-mM ammonium acetate; Gradient: 40-100% B over 15 minutes, then a 5-minute hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dried via centrifugal evaporation to give Example 39 (13.2 mg, 62% yield). LC/MS (M+18): 600.1; LC retention time: 2.296 (analytical HPLC Method B); 1H NMR (500 MHz, 1 : 1 mixture of CDCI3-CD3OD) delta ppm 7.56 (d, J=8.4 Hz, 2H), 7.50 – 7.41 (m, 1H), 7.38 – 7.30 (m, 2H), 7.19 (d, J=8.4 Hz, 2H), 7.11 – 6.97 (m, 4H), 4.70 (s, 2H), 3.27 (ddd, J=13.9, 9.9, 5.9 Hz, 2H), 2.81 – 2.67 (m, 2H), 2.45 – 2.30 (m, 1H), 2.13 – 1.97 (m, 1H).

The synthetic route of 627-31-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; DUAN, Jingwu; DHAR, T. G. Murali; JIANG, Bin; LU, Zhonghui; KARMAKAR, Ananta; GUPTA, Arun Kumar; WEIGELT, Carolyn A.; WO2015/103508; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 627-31-6, These common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

EXAMPLE 3 STR18 3-acetylthiopropyliodide (10) To a solution of 1,3-diiodopropane (10 g, 33.8 mmol) in 10 ml of anhydrous DMF at 0 C. under nitrogen is added, via a cannula over 15 min, a solution of potassium thioacetate (1.3 g, 11.3 mmol) in 5 ml of DMF and the mixture is stirred at 0 C. for 0.5 h, quenched with water (20 ml) and extracted with ether (3*20 ml). The extracts are combined, washed with brine and dried over MgSO4, filtered and concentrated. The residue is purified by flash chromatography (silica gel, EtOAc:hexane/5:95-10:90) to yield iodide 10 (2.5 g, 90%) as a light yellow oil. IR (neat) 2960, 2920, 1689, 1418, 1350, 1210, 1130 cm-1; 1 H NMR (CDCl3) delta 2.00 (2H, m), 2.26 (3H, s), 2.87 (2H, t, J=7 Hz), 3.13 (2H, t, J=6.9 Hz); 13 C NMR (CDCl3) delta 4.35, 29.70, 30.63, 32.97, 195.09.

The synthetic route of 627-31-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck Frosst Canada & Co.; US6121253; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com