Ammonia → Nordiazepam

HRID 1973066

反応式

HRID 1973066 の反応式
C1N2CN3CN(C2)C[N:2]1C3.Cl[CH2:12][C:13]([NH:15][C:16]1[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][C:17]=1[C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=O)=[O:14].N>CO>[Cl:30][C:27]1[CH:28]=[CH:29][C:16]2[NH:15][C:13](=[O:14])[CH2:12][N:2]=[C:18]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:17]=2[CH:26]=1

参加物

5

反応物 3

HCID 222Ammonia3 回HCID 4101HexamethylenetetramineHCID 776355-Chloro-2-(chloroacetamido)benzophenone

生成物 1

HCID 2997Nordiazepam収率 624.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of methanol (550 mls), hexamethylenetetramine (14.1 g., 0.1 mol) and 2-chloroacetamido-5-chlorobenzophenone (308.2 g., 1.0 mol) was stirred and saturated with ammonia at room temperature. The mixture was heated slowly to reflux with a steady stream of ammonia bubbling through the solution. Refluxing was continued for 24 hours. The flow of ammonia was interrupted and the crystal slurry obtained was cooled to room temperature. The product, filtered, washed with methanol (2 × 125 ml) and hot water (4 × 500 ml), and dried gave 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (169 g., 62.3%) melting at 213° to 215° C.

後処理

  1. temperatureThe mixture was heated slowly
  2. temperatureRefluxing
  3. customthe crystal slurry obtained
  4. filtrationThe product, filtered
  5. washwashed with methanol (2 × 125 ml) and hot water (4 × 500 ml)
  6. customdried

出典と根拠

ORDレコード
ord-57f62855293a4e2eb21841d79ab5dc2c
出典データセット
uspto-grants-1976_12
特許番号
US03996209

関連ノート

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