Phosgene → HCID 13742718, 화합물

HRID 1733143노트

반응식

HRID 1733143 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:6]=1[C:7]#[N:8].[C:13](Cl)(Cl)=[O:14].C[C@H]1CO[C@@]2(O[C@H]3C[C@H]4[C@@H]5CC=C6C[C@@H](O)CC[C@]6(C)[C@H]5CC[C@]4(C)[C@H]3[C@@H]2C)CC1>ClC1C=CC=CC=1>[C:7]([C:6]1[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][S:3][C:2]=1[N:1]=[C:13]=[O:14])#[N:8]

참가 물질

5

반응물 3

HCID 6371Phosgene3회HCID 99474DiosgeninHCID 5968662-Amino-4-(1,1-dimethylethyl)-3-thiophenecarbonitrile

생성물 1

HCID 13742718HCID 13742718, 화합물수율 60.1%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매2회

실험 절차

A solution of 90 g (0.5 mole) of 2-amino-3-cyano-4-tert.-butyl-thiophene in 300 ml of chlorobenzene was added dropwise to a solution of 150 g of phosgene in 1.5 liters of chlorobenzene at 0°-5° C. Thereafter, the mixture was slowly heated to the boil, while passing further phosgene in, and excess phosgene was then driven off by passing dry nitrogen in. For working up, the solvent was stripped off under reduced pressure and the residue was distilled. 62 g of 3-cyano-4-tert.-butyl-thien-2-yl isocyanate, which boiled at 163° C. under a pressure of 20 mm Hg, were obtained in this manner.

후처리

  1. temperatureThereafter, the mixture was slowly heated to the boil
  2. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-24e22ecf6aa34398bd29d444aced0dc2
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04240820

반응 노트

불러오는 중…