Water → HCID 23368486, 화합물

HRID 1901611노트

반응식

HRID 1901611 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].[CH3:24][N:25]=[C:26]=[O:27].O.C(OCC)(=O)C>CN(C)C=O.C(Cl)Cl>[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:22][O:23][C:26]([NH:25][CH3:24])=[O:27])[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]

참가 물질

7

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 12228Methyl IsocyanateHCID 233683553-(2-Tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole

생성물 1

HCID 23368486HCID 23368486, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.50 g of 3-(2-tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole in 5 ml of N,N-dimethylformamide is added 0.14 g of cuprous chloride. To this solution is added a solution of 0.13 g of methyl isocyanate in 5 ml of methylene chloride at 20°-25° C., and they are further subjected to reaction at the same temperature for 30 minutes. Water and ethyl acetate are added to the reaction mixture, and after shaking, the organic layer is separated. The separated organic layer is washed with water and a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure, to obtain 3-(2-tert-butoxycarbonylamino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole.

후처리

  1. customthey are further subjected to reaction at the same temperature for 30 minutes
  2. customthe organic layer is separated
  3. washThe separated organic layer is washed with water
  4. dry with materiala saturated saline solution and dried over anhydrous magnesium sulfate
  5. customafter which the solvent is removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-4906bb6f3de74eb9b6fc5a1817adbd65
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05578627

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