反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]12[O:25][CH2:24][CH2:23][N:9]1[CH2:10][C:11](=[O:22])[NH:12][C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][C:14]=12.[H-].[Na+].Br[CH2:29][CH2:30][OH:31]>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]12[O:25][CH2:24][CH2:23][N:9]1[CH2:10][C:11](=[O:22])[N:12]([CH2:29][CH2:30][OH:31])[C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][C:14]=12参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of 1.5 g (0.0041 M) of 11b-(2-chlorophenyl)-10-nitro-2,3,5,11b-tetrahydrooxazolo [3,2-d][1,4]benzodiazepin-6(7H)-one in 30 ml of dry N,N-dimethylformamide was treated with 0.34 g (0.008 M) of a 57% dispersion of sodium hydride in mineral oil with stirring under nitrogen. After 30 min, 1.5 g (0.012 M) of 2-bromoethanol was added and the reaction was heated to 90° for 3 hr. The solvent was removed under vacuum, and the residue was dissolved in 50 ml of dichloromethane which was then washed with 50 ml of water, 25 ml of a saturated solution of brine, dried over anhydrous sodium sulfate and evaporated to dryness. The residue was crystallized from ether, and recrystallized from a mixture of dichloromethane and methanol to give the product as pale yellow prisms, m.p. 185°-190° (dec.).
後処理
- temperaturethe reaction was heated to 90° for 3 hr
- customThe solvent was removed under vacuum
- dissolutionthe residue was dissolved in 50 ml of dichloromethane which
- washwas then washed with 50 ml of water, 25 ml of a saturated solution of brine
- dry with materialdried over anhydrous sodium sulfate
- customevaporated to dryness
- customThe residue was crystallized from ether
- customrecrystallized from a mixture of dichloromethane and methanol
出典と根拠
- ORDレコード
- ord-b0b3e6cb9a704834817d98b9a9ecade8
- 出典データセット
- uspto-grants-1976_12
- 特許番号
- US03997591
関連ノート
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