Ammonia → HCID 23368381、化合物

HRID 1901608ノート

反応式

HRID 1901608 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:22][OH:23])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:24](=[O:29])=[N:25][C:26](Cl)=[O:27].CO.[NH3:32]>C(Cl)Cl.O>[NH:25]([C:24]([O:23][CH2:22][CH:9]([NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1)=[O:29])[C:26]([NH2:32])=[O:27]

参加物

7

反応物 4

HCID 222AmmoniaHCID 887MethanolHCID 119708Isocyanatocarbonyl chlorideHCID 233683553-(2-Tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole

生成物 1

HCID 23368381HCID 23368381、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 1.00 g of 3-(2-tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole in 5 ml of methylene chloride is added to a solution of 0.31 g of N-(chlorocarbonyl) isocyanate in 10 ml of methylene chloride at -50° to -40° C. This solution is added to 10 ml of a methanol solution (8.0N) of ammonia at -20° C. over 20 minutes, and the temperature is elevated to 0° C., at which they are subjected to reaction for 30 minutes. Water is added to the reaction mixture, and after shaking, the organic layer is separated. The separated organic layer is washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure, to obtain 3-(3-ureidocarbonyloxy-2-tert-butoxycarbonylaminopropoxy)-5-chloro-1,2-benzoisoxazole.

後処理

  1. customis elevated to 0° C., at which they
  2. customare subjected to reaction for 30 minutes
  3. customthe organic layer is separated
  4. washThe separated organic layer is washed with a saturated saline solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customafter which the solvent is removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-cf243cba3d204ff8bcb18a3ccb284af1
出典データセット
uspto-grants-1996_11
特許番号
US05578627

反応ノート

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