Sodium Methoxide → 7-Chloro-2-methoxy-5-phenyl-3H-1,4-benzodiazepine

HRID 649262

반응식

HRID 649262 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([O:12]P(N3CCOCC3)(N3CCOCC3)=O)[CH2:9][N:8]=[C:7]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:33]=1.[CH3:34][O-].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([O:12][CH3:34])[CH2:9][N:8]=[C:7]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:33]=1

참가 물질

4

실험 절차

To a solution of 24.5 mg. (0.5 mmoles) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepine in 5 ml. of methanol at room temperature was added 82 mg. (1.5 mmoles) of sodium methoxide. The mixture was left at room temperature overnight. Methanol was evaporated and the residue was slurried with ether. Insoluble salts were removed by filtration. The clear ether solution was evaporated. Crystallization of the residue from petroleum ether yielded a final product having a m.p. of 94°-97°.

후처리

  1. customMethanol was evaporated
  2. customInsoluble salts were removed by filtration
  3. customThe clear ether solution was evaporated
  4. customCrystallization of the residue from petroleum ether

출처 및 근거

ORD 기록
ord-17f948a8d4fd4ffc89a4c301235b8fc8
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04739049

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