Water → 7-chloro-N-(2-chloroethyl)-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide 4-oxide

HRID 1706615노트

반응식

HRID 1706615 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12]([NH:14][CH2:15][CH2:16][Cl:17])=[O:13])[CH2:10][CH2:9][N:8]=[C:7]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:24])[C:6]=2[CH:25]=1.[OH2:26]>C(O)(=O)C.C(OO)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12]([NH:14][CH2:15][CH2:16][Cl:17])=[O:13])[CH2:10][CH2:9][N+:8]([O-:26])=[C:7]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:24])[C:6]=2[CH:25]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 20333751HCID 20333751, 화합물

생성물 1

HCID 203337717-chloro-N-(2-chloroethyl)-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide 4-oxide

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6585Peracetic Acid용매

실험 절차

10 Parts of 7-chloro-N-(2-chloroethyl)-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide is dissolved in 50 parts by volume of glacial acetic acid and to this solution 10 parts by volume of 40% peracetic acid is added all at once with stirring. The reaction mixture is stirred at ambient temperature for about 24 hours and then slowly poured into 1000 parts by volume of cold water. The precipitate which forms is extracted with methylene chloride, the extract dried over magnesium sulfate and the solvent removed. The residue crystallizes from ethanol to afford 7-chloro-N-(2-chloroethyl)-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide 4-oxide. This compound is represented by the following formula ##STR37##

후처리

  1. additionis added all at once
  2. stirringThe reaction mixture is stirred at ambient temperature for about 24 hours
  3. extractionThe precipitate which forms is extracted with methylene chloride
  4. dry with materialthe extract dried over magnesium sulfate
  5. customthe solvent removed
  6. customThe residue crystallizes from ethanol

출처 및 근거

ORD 기록
ord-d7ec9b7d409e4e5e9553896633efeee1
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04208327

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