Water → 3-(3-Carbamoyloxy-2-tert-butoxycarbonylaminopropoxy)-5-chloro-1,2-benzoisoxazole

HRID 1901603노트

반응식

HRID 1901603 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].ClS([N:28]=[C:29]=[O:30])(=O)=O.O>C(Cl)Cl>[C:29]([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:30])[NH2:28]

참가 물질

5

반응물 3

HCID 962WaterHCID 70918Chlorosulfonyl isocyanateHCID 233683553-(2-Tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole

생성물 1

HCID 233685643-(3-Carbamoyloxy-2-tert-butoxycarbonylaminopropoxy)-5-chloro-1,2-benzoisoxazole수율 85.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 3.43 g of 3-(2-tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole in 34 ml of methylene chloride is added 1.70 g of chlorosulfonyl isocyanate at -45° to -40° C., and the temperature thereof is elevated to 0° C., after which they are subjected to reaction at the same temperature for one hour. To the reaction mixture is added 10 ml of water and they are subjected to reaction at 20°-25° C. for one hour, after which methylene chloride is removed by distillation under reduced pressure. The crystals obtained are collected by filtration, to obtain 3.30 g of 3-(3-carbamoyloxy-2-tert-butoxycarbonylaminopropoxy)-5-chloro-1,2-benzoisoxazole.

후처리

  1. customthereof is elevated to 0° C.
  2. customafter which they are subjected to reaction at the same temperature for one hour
  3. customare subjected to reaction at 20°-25° C. for one hour
  4. customafter which methylene chloride is removed by distillation under reduced pressure
  5. customThe crystals obtained
  6. filtrationare collected by filtration

출처 및 근거

ORD 기록
ord-6c0cf16dae814ead89507946b2d0d23f
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05578627

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