Water → HCID 23368486、化合物

HRID 1901611ノート

反応式

HRID 1901611 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].[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]

参加物

7

反応物 4

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

生成物 1

HCID 23368486HCID 23368486、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4906bb6f3de74eb9b6fc5a1817adbd65
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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