Benzyl Bromide → HCID 18940592、化合物

HRID 356145ノート

反応式

HRID 356145 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]1[CH2:9][C:8](=[O:10])[NH:7][C:6]2[CH:11]=[CH:12][CH:13]=[CH:14][C:5]=2[N:4]=1.[H-].[Na+].[CH2:19](Br)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C)C=O.O>[CH2:19]([N:7]1[C:6]2[CH:11]=[CH:12][CH:13]=[CH:14][C:5]=2[N:4]=[C:3]([C:2]([F:1])([F:15])[F:16])[CH:9]([CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:8]1=[O:10])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

参加物

6

反応物 3

HCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 5357161,3-Dihydro-4-(trifluoromethyl)-2H-1,5-benzodiazepin-2-one

生成物 1

HCID 18940592HCID 18940592、化合物収率 61.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-trifluoromethyl-1,3-dihydro-1,5-benzodiazepin-2(2H)-one(3.0 g, 13.1 mmol) in N,N-dimethylformamide(20 mL) was added sodium hydride (content 60%, 1.1 g, 27.5 mmol), and the mixture was stirred for 15 minutes. To the mixture was added benzyl bromide (4.7 g, 27.5 mmol), which was stirred for further 30 minutes. The reaction mixture was diluted with water, which was extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The concentrate was crystallized from ethyl acetate-hexane to give 3.3 g of the titled compound. Yield 61%. m.p. 150°-151° C.

後処理

  1. stirringwas stirred for further 30 minutes
  2. extractionwas extracted with ethyl acetate
  3. washThe extract was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe concentrate was crystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-fd33974249bc46cca45587119625ffa6
出典データセット
uspto-grants-1998_11
特許番号
US05834463

反応ノート

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