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

HRID 1901603ノート

反応式

HRID 1901603 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].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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6c0cf16dae814ead89507946b2d0d23f
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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