HRID444265

反应详情

EQUATION

反应方程式

HRID 444265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 2-hydroxyimino-2-(isothiazol-4-yl)acetate (anti isomer) (3.41 g.), 36% aqueous solution of formaldehyde (24 ml.), conc. hydrochloric acid (12 ml.) and water (24 ml.) was stirred for 7 hours at 90° to 100° C. The reaction mixture was allowed to stand overnight in a refrigerator to precipitate crystals. The crystals were collected by filtration, washed with a small amount of ice-water and then dried to give 2-(isothiazol-4-yl)glyoxylic acid (2.09 g.). The mother liquor was extracted with ethyl acetate to give the same compound (0.34 g.), mp 145° to 148° C.

WORKUP

后处理

  1. waitto stand overnight in a refrigerator
  2. customto precipitate crystals
  3. filtrationThe crystals were collected by filtration
  4. washwashed with a small amount of ice-water
  5. customdried