Sodium Hydroxide → HCID 23318332、化合物

HRID 1981974ノート

反応式

HRID 1981974 の反応式
[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

参加物

5

反応物 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

生成物 1

HCID 23318332HCID 23318332、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-847b2a73de7243b3981f322096bdc0be
出典データセット
uspto-grants-1986_06
特許番号
US04594436

反応ノート

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