Sodium Hydroxide → HCID 23318332, 화합물

HRID 1980245노트

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HRID 1980245 반응식
[CH3:1][N:2]1[CH2:23][CH2:22][N:5]2[C:6]3[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:7]=3[C:8]([C:12]3[O:13][CH:14]=[CH:15][CH:16]=3)=[N+:9]([O-])[CH2:10][CH:4]2[CH2:3]1.P(Cl)(Cl)[Cl:25].[OH-].[Na+]>C(Cl)(Cl)Cl>[CH3:1][N:2]1[CH2:23][CH2:22][N:5]2[C:6]3[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:7]=3[C:8]([C:12]3[O:13][C:14]([Cl:25])=[CH:15][CH:16]=3)=[N:9][CH2:10][CH:4]2[CH2:3]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24387Phosphorus trichlorideHCID 30712577-(Furan-2-yl)-3,9-dimethyl-6-oxo-1,2,3,4,4a,5-hexahydro-6lambda~5~-pyrazino[1,2-a][1,4]benzodiazepine

생성물 1

HCID 23318332HCID 23318332, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

9.3 g of 1,2,3,4,4a,5-hexahydro-3,9-dimethyl-7-(2-furyl)-pyrazino[1,2-a][1,4]benzodiazepine 6-oxide (prepared analogously to Example 5) are heated under reflux in 150 ml of chloroform with 17 ml of phosphorus trichloride for 1 hour. The reaction mixture is then treated with aqueous sodium hydroxide solution and worked up. The resulting crude product is separated into its components by chromatography on aluminium oxide of activity level II, using methylene chloride/chloroform. 1.7 g of the less polar 1,2,3,4,4a,5-hexahydro-3,9-dimethyl-7-(5-chloro-2-furyl)-pyrazino[1,2-a][1,4]benzodiazepine are thereby initially obtained in the first fraction, and the product is isolated as an oil (IR: 1,615 cm-1C=N) (b). 5 g of the more highly polar 1,2,3,4,4a,5-hexahydro-3,9-dimethyl-7-(2-furyl)-pyrazino[1,2-a][1,4]benzodiazepine (a) are then obtained.

후처리

  1. temperatureare heated
  2. customThe resulting crude product is separated into its components by chromatography on aluminium oxide of activity level II

출처 및 근거

ORD 기록
ord-847c91eba04f4ed296b79e6ad62d43ff
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04508716

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