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

HRID 649262

反応式

HRID 649262 の反応式
[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

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 149078867-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin

生成物 1

HCID 6249427-Chloro-2-methoxy-5-phenyl-3H-1,4-benzodiazepine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-17f948a8d4fd4ffc89a4c301235b8fc8
出典データセット
uspto-grants-1988_04
特許番号
US04739049

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