Ethanol → 7-Chloro-5-(2'-chloro-phenyl)-1,3-dihydro-3-(dimethylaminomethylene)-2H-1,4-benzodiazepin-2-one

HRID 1076389노트

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HRID 1076389 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1.C(O)C.C(O[CH:27](OCC)[N:28]([CH3:30])[CH3:29])C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[C:9](=[CH:27][N:28]([CH3:30])[CH3:29])[N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 17925DelorazepamHCID 70913Dimethylformamide diethylacetal

생성물 1

HCID 1363535337-Chloro-5-(2'-chloro-phenyl)-1,3-dihydro-3-(dimethylaminomethylene)-2H-1,4-benzodiazepin-2-one

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온도
130 °C

실험 절차

A suspension of 50 gm of 7-chloro-5-(2'-chlorophenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one in 100 ml of N,N-dimethyl-formamide diethylacetal was heated to 130°C in a vessel equipped with a descending condenser, whereby a clear solution was formed after a short time. The temperature of the reaction solution was maintained at 130°C for 40 minutes, during which time the ethanol formed by the reaction slowly distilled over. Thereafter, the reaction solution was allowed to cool, and the red precipitate was collected by vacuum filtration, washed with petroleum ether and recrystallized from methanol, whereupon it had a melting point of 239°-241°C. It was identified to be the compound of the formula ##SPC6##

후처리

  1. customequipped with a descending condenser
  2. customwhereby a clear solution was formed after a short time
  3. customformed by the reaction
  4. distillationslowly distilled over
  5. temperatureto cool
  6. filtrationthe red precipitate was collected by vacuum filtration
  7. washwashed with petroleum ether
  8. customrecrystallized from methanol, whereupon it

출처 및 근거

ORD 기록
ord-7f87dbed62cc469cb7913123ec3770ae
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03956492

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