Water → HCID 23368486, Verbindung

HRID 1901611Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1901611
[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]

Komponenten

7

Edukt 4

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

Produkt 1

HCID 23368486HCID 23368486, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-4906bb6f3de74eb9b6fc5a1817adbd65
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05578627

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