Ammonia → HCID 23368381, 화합물

HRID 1901608노트

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HRID 1901608 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 23368381HCID 23368381, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cf243cba3d204ff8bcb18a3ccb284af1
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05578627

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