Phosgene → HCID 13742718、化合物

HRID 1733143ノート

反応式

HRID 1733143 の反応式
[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]

参加物

5

反応物 3

HCID 6371Phosgene3 回HCID 99474DiosgeninHCID 5968662-Amino-4-(1,1-dimethylethyl)-3-thiophenecarbonitrile

生成物 1

HCID 13742718HCID 13742718、化合物収率 60.1%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-24e22ecf6aa34398bd29d444aced0dc2
出典データセット
uspto-grants-1980_12
特許番号
US04240820

反応ノート

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