Tag: M.W=300-400

628-21-7, Adding a certain compound to certain chemical reactions, such as: 628-21-7, name is 1,4-Diiodobutane, 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 628-21-7.

To a solution of 500 mg (2.16 mmol) of L-serine benzyl ester hydrochloride and 869 mg (2.81 mmol, 1.3 eq.) of 1,4-diiodobutane in 25 ml of 2-propanol were added, under argon at RT, 595 mg (5.61 mmol, 2.6 eq.) of sodium carbonate and the mixture was stirred at 90 C. overnight. After cooling to RT and removal of the 2-propanol under reduced pressure, the residue was admixed with ethyl acetate. The insoluble salts were filtered off. The filtrate was washed with water and the organic phase was dried (sodium sulphate), filtered and concentrated under reduced pressure. The residue was purified by means of flash chromatography (silica gel 50, dichloromethane, then dichloromethane/methanol 5:1). Yield: 268 mg (48% of theory) LC/MS [Method 5]: Rt=2.03 min; MS (ESIpos): m/z=250 (M+H)+.

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; ROeHRIG, Susanne; HILLISCH, Alexander; HEITMEIER, Stefan; SCHMIDT, Martina Victoria; SCHLEMMER, Karl-Heinz; TERSTEEGEN, Adrian; TELLER, Henrik; US2018/346424; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

672-57-1, 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. 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below.

1 4-(2-Chloro-5-trifluoromethylphenyl)-1-fluoro-2-fluoromethyl-3-butyn-2-ol A mixture of 4-chloro-3-iodobenzotrifluoride (63.3 g), 1-fluoro-2-fluoromethyl-3-butyn-2-ol (28.8 g), triethylamine (26.2 g), cuprous iodide (0.38 g), bis(triphenylphosphine)palladium chloride (1.40 g) and N,N-dimethylformamide (100 ml) was stirred under a nitrogen atmosphere under heating at 80 C. for 1.5 hours. To the reaction mixture, 2 N HCl and a hexane/ethyl acetate mixed solvent (3/1) were added and the insoluble matter was filtered off with Celite; following extraction with a hexane/ethyl acetate mixed solvent (3/1), the resulting organic layers were combined, washed with a saturated aqueous solution of sodium chloride, dried with anhydrous sodium sulfate and concentrated under reduced pressure; the resulting residue was purified by distillation to give 4-(2-chloro-5-trifluoromethylphenyl)-1-fluoro-2-fluoromethyl-3-butyn-2-ol (44.5 g) having a boiling point of 105-107 C./1 mmHg. 1H-NMR (CDCl3) delta: 2.70-3.00(1H, m), 4.52-4.71(4H, m), 7.54-7.56(2H, m), 7.76(1H, t, J=0.7 Hz)

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; Chugai Seiyaku Kabushiki Kaisha; US6455708; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

n-Butyl lithium (2.5 M in hexanes, 4.2 mL, 0.5 mmol) was added dropwise to a suspension of indolinone (0.665 mg, 5 mmol) and TMEDA (1.5 mL, 10 mmol) in THF (20 mL) at -78C in a dried flask under nitrogen. After 1 hour at -78C, 1,4- diiodobutane (3.3 mL, 25 mmol) was added dropwise and the mixture was allowed to slowly warm to rt. After 12 hours at rt, saturated aqueous ammonium chloride was added to the mixture and this mixture was extracted with EtOAc. The combined organic phases were washed with water, brine, dried over magnesium sulphate, filtered and concentrated in vacuo. Chromatography on silica (10-30% EtOAc in isohexane) gave isolation of the desired compound as a pale pink solid (393 mg, 2.1 mmol, 42%). ? NMR (400 MHz): delta 1.90 (m, 2H), 2.03 (m, 2H), 2.10 ( m, 2H), 2.21 (m, 2H), 6.94 ( m, 1H), 7.04 ( m, 1H), 7.20 (m, 2H), 8.75 ( bs, 1H). LC/MS 188 (MH+).

The synthetic route of 1,4-Diiodobutane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RE:VIRAL LTD; COCKERILL, Stuart; PILKINGTON, Christopher; LUMLEY, James; ANGELL, Richard; MATHEWS, Neil; WO2013/68769; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, Adding a certain compound to certain chemical reactions, such as: 628-21-7, name is 1,4-Diiodobutane, 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 628-21-7.

Into a 100 ml flask to which a condensing device was connected, 50 ml of acetonitrile, 15.5 g (0.05 mol) of 1,4-diiodobutane and 6.8 g of aqueous ammonia (NH3 0.1 mol) were added. 20C constant temperature stirring reaction 12h. The obtained reaction solution was subjected to cation chromatography. According to the product content in the reaction solution. The yield was calculated to be 85.35%.

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Changshu Institute Co., Ltd., East China University of Science and Technology; East China University of Science and Technology; Guan, Shiyou; Feng, Lei; Xiong, Yachao; Yan, Xinzhu; (16 pag.)CN105732645; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 629-09-4 name is 1,6-Diiodohexane, 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. 629-09-4

To a suspension of potassium 1,3-dioxoisoindolin-2-ide (5 g, 27 mmol) in DMF (250 mL) was added 1,6-diiodohexane (22.83 g, 67.5 mmol) dropwise and heated at 85 C for 2 h. The reaction mixture was monitored with LCMS. The reaction mixture was diluted with cold water and extracted with diethyl ether (2×300 mL), and the combined organic layer was washed with water (3×250 mL) and brine (250 mL). The organic layer dried over sodium sulfate and concentrated under reduced pressure to obtain a crude product which was purified by column chromatography with 10% EtOAc in hexane as eluent to afford 8.5 g of 2-(6- iodohexyl)isoindoline- 1 ,3-dione.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,6-Diiodohexane, and friends who are interested can also refer to it.

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

Some common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, molecular formula is C6H3BrINO2, 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. 112671-42-8

(3) Add (100mmol) M2 to the reaction flask32.6g (100mmol) of 2-iodo-5-bromonitrobenzene,(1%) Pd (PPh3) 4,40g (300mmol) sodium carbonate,Toluene (800mL), ethanol (200mL)And water (200mL),Heated to reflux, reacted for 8h, the reaction was completed;The reaction solution was extracted with ethyl acetate, and the organic phase was concentrated.A yellow solid M3 was obtained;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 112671-42-8, its application will become more common.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (28 pag.)CN110698458; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 628-21-7, name is 1,4-Diiodobutane, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 628-21-7

Preparatory Example 7 Spiro[cyclopentane-1,3′-indolin]-2′-one n-Butyl lithium (2.5 M in hexanes, 4.2 mL, 0.5 mmol) was added dropwise to a suspension of indolinone (0.665 mg, 5 mmol) and TMEDA (1.5 mL, 10 mmol) in THF (20 mL) at -78 C. in a dried flask under nitrogen. After 1 hour at -78 C., 1,4-diiodobutane (3.3 mL, 25 mmol) was added dropwise and the mixture was allowed to slowly warm to rt. After 12 hours at rt, saturated aqueous ammonium chloride was added to the mixture and this mixture was extracted with EtOAc. The combined organic phases were washed with water, brine, dried over magnesium sulphate, filtered and concentrated in vacuo. Chromatography on silica (10-30% EtOAc in isohexane) gave isolation of the desired compound as a pale pink solid (393 mg, 2.1 mmol, 42%). 1H NMR (400 MHz): delta 1.90 (m, 2H), 2.03 (m, 2H), 2.10 (m, 2H), 2.21 (m, 2H), 6.94 (m, 1H), 7.04 (m, 1H), 7.20 (m, 2H), 8.75 (bs, 1H). LC/MS 188 (MH+).

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, 628-21-7, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; re: Viral Ltd; Cockerill, Stuart; Pilkington, Christopher; Lumley, James; Angell, Richard; Mathews, Neil; US2014/308282; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

364-12-5, The chemical industry reduces the impact on the environment during synthesis 364-12-5, name is 5-Bromo-2-iodobenzotrifluoride, I believe this compound will play a more active role in future production and life.

(1) Synthesis of 1-[4-bromo-2-(trifluoromethyl)phenyl]cyclobutanol To a solution of 5-bromo-2-iodobenzotrifluoride (5.00 g) in dehydrated tetrahydrofuran (140 mL), n-butyl lithium (2.69 mol/L, solution in n-hexane, 5.30 mL) was added at -78C and the mixture was stirred at that temperature for 25 minutes. After adding a solution of cyclobutanone (999 mg) in tetrahydrofuran (5.00 mL), the mixture was brought to room temperature and stirred for 3 days. After adding a saturated aqueous solution of ammonium chloride under cooling with ice, two extractions were conducted with ethyl acetate. The combined organic layers were washed with water and thereafter dried over anhydrous magnesium sulfate. After removing the desiccant by filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate = 98:2-80:20) to give 1-[4-bromo-2-(trifluoromethyl)phenyl]cyclobutanol as a pale yellow oil (3.00 g). 1H NMR (300 MHz, CHLOROFORM-d) delta ppm 1.71 – 1.88 (m, 1 H) 2.20 – 2.49 (m, 3 H) 2.52 – 2.70 (m, 2 H) 7.29 – 7.35 (m, 1 H) 7.62 – 7.69 (m, 1 H) 7.78 – 7.84 (m, 1 H). MS EI posi: 294[M]+.

The chemical industry reduces the impact on the environment during synthesis 5-Bromo-2-iodobenzotrifluoride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Taisho Pharmaceutical Co., Ltd.; TAKAYAMA, Tetsuo; SHIBATA, Tsuyoshi; SHIOZAWA, Fumiyasu; KAWABE, Kenichi; SHIMIZU, Yuki; HAMADA, Makoto; HIRATATE, Akira; TAKAHASHI, Masato; USHIYAMA, Fumihito; OI, Takahiro; SHIRASAKI, Yoshihisa; MATSUDA, Daisuke; KOIZUMI, Chie; KATO, Sota; EP2881384; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com