Chloroacetyl isocyanate → 7-chloro-N-chloracetyl-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide

HRID 1706613노트

반응식

HRID 1706613 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH2:10][CH2:9][N:8]=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:18])[C:6]=2[CH:19]=1.[Cl:20][CH2:21][C:22]([N:24]=[C:25]=[O:26])=[O:23]>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:25]([NH:24][C:22](=[O:23])[CH2:21][Cl:20])=[O:26])[CH2:10][CH2:9][N:8]=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:18])[C:6]=2[CH:19]=1

참가 물질

4

반응물 2

HCID 78209Chloroacetyl isocyanateHCID 20333776HCID 20333776, 화합물

생성물 1

HCID 203337737-chloro-N-chloracetyl-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The mixture of 8 parts of 7-chloro-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine, 4.9 parts of chloroacetylisocyanate, and 200 parts by volume of methylene chloride is stirred under nitrogen atmosphere at ambient temperature for about one hour. The mixture is then filtered through a layer of activated magnesium silicate and the filtrate evaporated to dryness. The resultant yellow oil is dissolved in ether and the solvent removed by evaporation to give gummy residue which upon crystallization from ether affords 7-chloro-N-chloracetyl-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide, as a yellow solid melting at about 152°-156° C. This compound is represented by the following formula ##STR21##

후처리

  1. filtrationThe mixture is then filtered through a layer of activated magnesium silicate
  2. customthe filtrate evaporated to dryness
  3. dissolutionThe resultant yellow oil is dissolved in ether
  4. customthe solvent removed by evaporation
  5. customto give gummy residue which
  6. customupon crystallization from ether

출처 및 근거

ORD 기록
ord-380e3946dc8e4869a061b8e7e1e53b64
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04208327

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