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

HRID 1706615ノート

反応式

HRID 1706615 の反応式
[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

参加物

5

反応物 2

HCID 962WaterHCID 20333751HCID 20333751、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 6585Peracetic Acid溶媒

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-d7ec9b7d409e4e5e9553896633efeee1
出典データセット
uspto-grants-1980_06
特許番号
US04208327

反応ノート

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