Category: 627-31-6

Application 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.

Step-d: 7′-methyl-5′-nitro spirolcyclobutane- 1.3′-indolin1-2′-one: To a stirred solution of 7-methyl-5-nitroindolin-2-one (0.45g, 2.3 mmol) in dry THF was added LiHMDS (7.02 mL, 3 eq) dropwise at 0C and stirred there for 15 min. Subsequently, 1, 3-diiodo propane (1.3 mL, 11.7 mmol) was added and the reaction mixture was stirred at 0C to RT for 2 h. The reaction mixture was quenched with IN HC1. The aqueous layer was extracted with ethyl acetate and washed with water and brine, dried over MgS04 and evaporated. The crude material was purified by column chromatography using 5 % ethyl acetate in hexanes as eluent to afford the title compound as a pale yellow solid (0.060 g, 10%). -NMR (400 MHz, DMSO- d6): 8 10.99 (bs, 1H), 8.29 (d, 8.01 (s, 1H), 2.45-2.41 (m, 4H), 2.28 (s, 3H), 2.25- 2.19 (m, 2H); ES-MS: m z 231.2 (M-H)

Statistics shows that 1,3-Diiodopropane(stabilized with Copper chip) is playing an increasingly important role. we look forward to future research findings about 627-31-6.

Reference:
Patent; ORION CORPORATION; UJJINAMATADA, Ravi Kotrabasaiah; HOSAHALLI, Subramanya; SAMAJDAR, Susanta; ABBINENI, Chandrasekhar; WO2015/92118; (2015); 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. Recommanded Product: 627-31-6

1,3-iodopropane (27.5g, 93mmol) and 3-methyl-3-hydroxymethyl-oxetane (3.1g, 31mmol), sodium hydroxide (20g, 500mmol) in water and hexane stir in two-phase system, with tetrabutylammonium bromide as phase transfer catalyst, the reaction for 0.5 hours under reflux.After completion of the reaction by extraction, purified by distillation under reduced pressure to give a colorless liquid.Yield: 62%.

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

Reference:
Patent; Suzhou Institute of Nano Rui Medical Technology Co., Ltd.; Zhao, Peng; Wu, Liangliang; Liu, Jing; Lin, Chao; Wenxue, Jun; (19 pag.)CN105523946; (2016); A;,
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.

To a suspension of potassium i,3-dioxoisoindoiin-2-ide (3 g, 16.2 mrnoi) in DMF (150 mL) was added 1,3-diiodopropane (4.2 rnL, 36.4 mmol) dropwise and heated at 85C for 2 h. The reaction mixture was monitored by LCMS, The reaction mixture was diluted with cold water and extracted with diethyl ether (2×250 mL). The combined organic layer was washed with water (3×200 mL) and brine (250 rnL), The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The crude product was purified by chromatography with 10% EtOAc in hexane as eluent to afford 3 g of 2-(3–iodopropyl) isoindoline-i,3-dione.

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.

Reference:
Patent; MEDIVATION TECHNOLOGIES, INC.; MCCULLAGH, Emma; BERNALES, Sebastian; HUNG, David; (451 pag.)WO2017/19833; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 627-31-6, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), This compound has unique chemical properties. The synthetic route is as follows.

A solution of methyl 2-(4-nitrophenyl)acetate (6 g, 31 mmol) in DMF (100 ml) was cooled to 0 C with an ice bath. NaH (60% in oil) (2.5 g, 63 mmol) was added portion wise. The resulting mixture was allowed to warm to RT and was stirred for 15 min at RT. After 15 min the mixture was cooled again to 0 C and 1,3-diiodopropane (6 ml, 52 mmol) was added drop wise. The resulting mixture was allowed to stir at 0 C for 30 min, and from 0 C to 10 C for 1.5 h. After 1.5 h the solution was cooled to 0 C and water was added. The reaction mixture was extracted 3 times with DCM. The combined organics were concentrated under reduced pressure and the residue was purified by flash chromatography on silica (120 g flash column, 0-20% EtOAc in hexane, 10 CV) to afford methyl 1-(4-nitrophenyl)cyclobutanecarboxylate.

The chemical industry reduces the impact on the environment during synthesis 1,3-Diiodopropane(stabilized with Copper chip). I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK SHARP & DOHME CORP.; MCGOWAN, Meredeth Ann; ACHAB, Abdelghani; FRADERA, Xavier; HAN, Yongxin; LI, Derun; LIM, Jongwon; LIU, Kun; SCIAMMETTA, Nunzio; WHITE, Catherine, M.; YU, Wensheng; ZHANG, Hongjun; ZHOU, Hua; (109 pag.)WO2019/74747; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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, Computed Properties of C3H6I2

To a solution of ethyl 2-(4-nitrophenyl)acetate (9.0 g, 43 mmol) in DMF (100 mL) was added NaH (3.6 g, 90 mmol, 60% in oil) at 0 C. Then the reaction mixture was allowed to warm to RT and stirred for 15 min. The mixture was cooled to 0 C again and 1,3- diiodopropane (10 mL, 89 mmol) was added. The resulting mixture was stirred at 0 C for 30 min, then warmed to RT and stirred at RT for 1 h. The reaction was diluted with NH4C1 (sat., 200 mL), extracted with EtOAc. The combined organic layers were washed with brine, dried over Na2S04i filtered and concentrated in vacuo to afford a residue, which was purified by column chromatography on silica gel (EtOAc in petroleum ether: 0 – 5% gradient) to give the title compound (I-D). lH NMR (400 MHz, CDC13) delta 8.23 – 8.12 (m, 2 H), 7.52 – 7.38 (m, 2 H), 4.18 – 4.04 (m, 2 H), 2.94 – 2.82 (m, 2 H), 2.57 – 2.45 (m, 2 H), 2.18- 2.04(m, 1 H), 2.00- 1.75 (m, 1H), 1.22 – 1.12 (m, 3 H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ZHOU, Hua; ACHAB, Abdelghani; FRADERA, Xavier; HAN, Yongxin; LI, Derun; MCGOWAN, Meredeth, A.; SCIAMMETTA, Nunzio; SLOMAN, David, L.; YU, Wensheng; (98 pag.)WO2019/27855; (2019); A1;,
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., Safety of 1,3-Diiodopropane(stabilized with Copper chip)

To a solution of ethyl 2-(4-nitrophenyl)acetate (9 g, 43 mmol) in DMF (100 mL) was added NaH (3.6 g, 90 mmol) (60% in oil) at 0 C. The reaction mixture was allowed to warm to RT and was stirred for 15 min. The mixture was cooled to 0 C and 1,3-diiodopropane (10 mL, 89 mmol) was added. The resulting mixture was stirred at 0 C for 30 min, then warmed to RT. After 1 h the reaction mixture was diluted with aqueous NH4C1 (200 mL), and was extracted with EtOAc (200 mLx3). The combined organics were washed with brine (1000 mL), dried over saturated Na2SC>4, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography (SiC , petroleum ether/ EtOAc =50: 1 to 40: 1) to afford ethyl 1-(4-nitrophenyl)cyclobutanecarboxylate.

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.; MCGOWAN, Meredeth Ann; ACHAB, Abdelghani; FRADERA, Xavier; HAN, Yongxin; LI, Derun; LIM, Jongwon; LIU, Kun; SCIAMMETTA, Nunzio; WHITE, Catherine, M.; YU, Wensheng; ZHANG, Hongjun; ZHOU, Hua; (109 pag.)WO2019/74747; (2019); A1;,
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., Safety of 1,3-Diiodopropane(stabilized with Copper chip)

Diiodopropane (0.295 g, 1.00 mmol, 5.0 eq) and potassium carbonate (0.028 g, 0.20 mmol, 1.0 eq) were added to a solution of the phenol 33 (0.100 g, 0.020 mmol, 1.0 eq) in dry acetone (5 mL). The reaction mixture was heated at 60C for 6 hours when LC/MS showed complete reaction. The reaction mixture was concentrated to dryness under reduced pressure and the residue was purified by flash chromatography (silica gel, 75/25 v/v n-hexane/EtOAc to 50/50 v/v n-hexane/EtOAc) to afford the product as a colourless oil (0.074 g, 56%). LC/MS (3.853 min (ES+)), m/z: 669.0 [M+H]+. 1H NMR (400 MHz, CDC13) delta 7.26 (s, 1H), 6.90 (s, 1H), 6.68 (s, 1H), 6.24 (d, 1H, / = 15.3 Hz), 5.87 (d, 1H, / = 8.9 Hz), 5.78 (m, 1H), 5.53 (m, 1H), 5.12 (m, 2H), 4.65 (m, 2H), 4.41 (m, 1H), 4.11 (m, 1H), 3.93 (s, 3H), 3.81 (m, 1H), 3.40 (t, 2H, / = 6.7 Hz), 3.05 (dd, 1H, / = 16.3, 10.1 Hz), 2.57 (m, 1H), 2.34 (m, 2H), 1.84 (d, 3H, / = 6.6 Hz), 0.92 (s, 9H), 0.28 (s, 3H), 0.26 (s, 3H).

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.

Reference:
Patent; MEDIMMUNE LIMITED; LLOYD, Christopher O.; MARWOOD, Rose; HOWARD, Philip; HARPER, III, John W.; HOLLINGSWORTH, Robert; KAMAL, Adeela; DIMASI, Nazzareno; GAO, Changshou; TOADER, Dorin; WANG, Fengjiang; GINGIPALLI, Lakshmaiah; WO2015/155345; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 627-31-6, A common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), molecular formula is C3H6I2, 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.

Sodium hydride 60% in oil (0.43 g, 10.7 mmol) was added to a suspension of Iota,Gamma trimethylenebisthymine (1.51 g, 5.1 mmol) in dimethyl sulfoxide (80 mL) and stirred overnight at 60-65 C. 1, 3-Diiodopropane (1.63 g, 4.8 mmol) was added to the reaction mixture and stirred for 3 days at 80 C to give a clear solution. The solvent was evaporated; the residual solid was washed with potassium carbonate aqueous solution (30 mL), methanol (20 mL), and diethyl ether (20 mL). The product in was purified by silica gel column using ethyl acetate/ methanol as eluents to give the cyclic compound, II as a white solid (0.204 g, 12% ). H NMR (600 MHz, CDC13, ppm) : 7.05 (s, 2H, C6-H), 4.07 (t, 3H, N3-CH2), 3.75 (t, 4H, N1-CH2), 2.15(t, 2H, N3- C-CH2), 1.98 (t, 2H, N1-C-CH2), 1.89 (s, 6H, C5-CH3); 13C NMR (150 MHz, CDC13): 164.11, 152.53, 141.21, 108.15, 51.20, 45.73, 28.20, 26.35, 10.35; Mass (APCI-Neg): 331.13 (M-H)

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.

Reference:
Patent; REGENTS OF THE UNIVERSITY OF MINNESOTA; VINCE, Robert; RAZA, Abbas; DREIS, Christine; WO2013/106728; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 627-31-6, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), This compound has unique chemical properties. The synthetic route is as follows.

Example 4General Procedure for the Preparation of Alkyl Ester IodidesAlkyl ester iodides were prepared via reaction between methyl 2-methylpropanoate and appropriate alkyl diodide in the presence of butylithium and diisopropylamine according to the following process: under inert atmosphere, N,N-diisopropylamine (1.1eq) was dissolved in tetrahydrofuran (10eq). To the solution cooled down to 0 C. was added n-butyllithium (1.1eq) drop by drop. The solution was then cooled to -70 C. before adding 2-methylpropanoic acid (1eq). The mixture was stirred at -70 C. for 15 minutes. The appropriate diiodated derivative (2eq) was added drop by drop at -70 C., and then the reaction mixture was gradually warmed to room temperature and stirred for 20 hours. The solution was then hydrolysed by adding HCl 2N to reach acidic pH. The aqueous layer was extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, filtered, and evaporated under reduced pressure. The residue was chromatographed over silica gel.Example 4.1 methyl 2,2-dimethyl-5-iodo-pentanoate Prepared following the general procedure previously described using methyl 2-methylpropanoate and 1,3-diiodopropane. The residue was chromatographed over silica gel (eluent cyclohexane). The product was obtained as a pale yellow oil. Yield: 79% Rf (cyclohexane/ethyl acetate 98/2): 0.32 NMR 1H (CDCl3): 1.20 (s, 6H); 1.62 (m, 2H); 1.78 (m, 2H); 3.15 (t, 2H, J=7 Hz); 3.69 (s, 2H).

The chemical industry reduces the impact on the environment during synthesis 1,3-Diiodopropane(stabilized with Copper chip). I believe this compound will play a more active role in future production and life.

Reference:
Patent; GENFIT; US2010/4159; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 627-31-6

To a suspension of potassium 1,3-dioxoisoindolin-2-ide (3 g, 16.2 mmol) in DMF (150 mL) was added 1,3-diiodopropane (4.2 mL, 36.4 mmol) dropwise and heated at 85C for 2 h. The reaction mixture was monitored by LCMS. The reaction mixture was diluted with cold water and extracted with diethyl ether (2×250 mL). The combined organic layer was washed with water (3×200 mL) and brine (250 mL). The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The crude product was purified by chromatography with 10% EtOAc in hexane as eluent to afford 3 g of 2-(3-iodopropyl) isoindoline-1,3-dione.

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.

Reference:
Patent; MEDIVATION TECHNOLOGIES, INC.; MCCULLAGH, Emma; BERNALES, Sebastian; HUNG, David; (415 pag.)WO2017/19822; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com