Ammonia → Nordiazepam

HRID 1973068

반응식

HRID 1973068 반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:7]=1[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=O)=[O:4].[NH3:21].C=O>CO>[Cl:20][C:17]1[CH:18]=[CH:19][C:6]2[NH:5][C:3](=[O:4])[CH2:2][N:21]=[C:8]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:7]=2[CH:16]=1

참가 물질

5

반응물 3

HCID 222Ammonia2회HCID 712FormaldehydeHCID 776355-Chloro-2-(chloroacetamido)benzophenone

생성물 1

HCID 2997Nordiazepam수율 77.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of methanol (275 ml.) and 2-chloroacetamido-5-chlorobenzophenone (154.2 g., 0.5 mol) was heated to reflux with a steady stream of ammonia bubbling in. At reflux 37% formaldehyde solution (237 ml) was fed in over ca. 40 minutes. The reaction mixture was then heated under reflux for 5 hours. The flow of ammonia was stopped and the slurry of crystals was cooled to room temperature, filtered, washed with methanol (2 × 125 ml), hot water (4 × 500 ml) and dried. There was obtained 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (104.6 g., 77.3%), melting at 211.5° to 214.5° C.

후처리

  1. temperaturewas heated
  2. customwas fed in over ca. 40 minutes
  3. temperatureThe reaction mixture was then heated
  4. temperatureunder reflux for 5 hours
  5. filtrationfiltered
  6. washwashed with methanol (2 × 125 ml), hot water (4 × 500 ml)
  7. customdried

출처 및 근거

ORD 기록
ord-ceee4bb1f8bd495ba1d76efda1f03daa
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996209

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