HRID2397598

反应详情

EQUATION

反应方程式

HRID 2397598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To 2.31 liters of DMF is added 479 grams (2.75 moles) of 3-(chloroacetamino)-5-methylisoxazole followed by 699 grams (2.9 moles) of sodium saccharin dihydrate. The mixture is heated to 100° C. and this temperature is maintained for 2 hours. The cooled reaction mixture is poured into 8 liters of water, filtered and the wet cake is recrystallized from 15 liters of ethanol to give 658 grams (74.8%) of 2,3,dihydro-N-(5-methyl-3-isoxazolyl)-3-oxo-1,2-benzisothiazole-2-acetamide 1,1-dioxide, mp 218°-220° C.; I.R. and NMR spectra are consistant with the structure.

WORKUP

后处理

  1. temperaturethis temperature is maintained for 2 hours
  2. customThe cooled reaction mixture
  3. filtrationfiltered
  4. customthe wet cake is recrystallized from 15 liters of ethanol