Ammonia → Nordiazepam

HRID 1973066

반응식

HRID 1973066 반응식
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

참가 물질

5

반응물 3

HCID 222Ammonia3회HCID 4101HexamethylenetetramineHCID 776355-Chloro-2-(chloroacetamido)benzophenone

생성물 1

HCID 2997Nordiazepam수율 624.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-57f62855293a4e2eb21841d79ab5dc2c
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996209

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