HRID1703723

反应详情

EQUATION

反应方程式

HRID 1703723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.15 g. (0.0155 mole) of 3-carbethoxy-4-hydroxy-2-methyl-2H-1,2-benzothiazine 1,1-dioxide, 1.3 g. (0.0155 mole) of 3-aminoisoxazole, and 500 ml. of xylene was refluxed for 24 hr. in a Soxhlet apparatus, the thimble of which contained 10 g. of Linde 4A molecular sieve. The mixture was cooled to 25° and the resulting crystalline precipitate was collected and washed with ether to give 3.2 g. of product, m.p. 235-240° dec. Recrystallization from 175 ml. of ethyl acetate gave 1.6 g. of material, m.p. 237-240° dec.

WORKUP

后处理

  1. additionA mixture of 4.15 g
  2. temperatureThe mixture was cooled to 25°
  3. customthe resulting crystalline precipitate was collected
  4. washwashed with ether
  5. customto give 3.2 g
  6. customRecrystallization from 175 ml
  7. customof ethyl acetate gave 1.6 g