Methyl Isocyanate → 2-(4-methylsemicarbazido)-5-o-chlorophenyl-7-ethyl-3H-thieno[2,3-e][1,4]diazepine

HRID 1658532노트

반응식

HRID 1658532 반응식
[CH3:1][N:2]=[C:3]=[O:4].[NH:5]([C:7]1[CH2:8][N:9]=[C:10]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[Cl:25])[C:11]2[CH:16]=[C:15]([CH2:17][CH3:18])[S:14][C:12]=2[N:13]=1)[NH2:6]>O1CCCC1>[CH3:1][NH:2][C:3](=[O:4])[NH:6][NH:5][C:7]1[CH2:8][N:9]=[C:10]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[Cl:25])[C:11]2[CH:16]=[C:15]([CH2:17][CH3:18])[S:14][C:12]=2[N:13]=1

참가 물질

4

반응물 2

HCID 12228Methyl IsocyanateHCID 124342992-hydrazino-5-o-chlorophenyl-7-ethyl-3H-thieno[2,3-e][1,4]diazepine

생성물 1

HCID 215278582-(4-methylsemicarbazido)-5-o-chlorophenyl-7-ethyl-3H-thieno[2,3-e][1,4]diazepine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1.1 ml of methyl isocyanate is added to a suspension of 5 g of 2-hydrazino-5-o-chlorophenyl-7-ethyl-3H-thieno[ 2,3-e] [1,4] diazepine in 100 ml of tetrahydrofuran, and the resulting mixture is stirred at room temperature for 2 hours. Then the reaction mixture is poured into ice water, and the precipitated crystals are collected by filtration, washed with water, dried, and recrystallized from a mixture of chloroform and ligroin to give 2-(4-methylsemicarbazido)-5-o-chlorophenyl-7-ethyl-3H-thieno[ 2,3-e][1,4]diazepine, melting at 213°-215° C.

후처리

  1. filtrationthe precipitated crystals are collected by filtration
  2. washwashed with water
  3. customdried
  4. customrecrystallized from a mixture of chloroform and ligroin

출처 및 근거

ORD 기록
ord-cbbed60c63024bfaaa743c0aa051ec72
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03965111

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