HRID443708

反应详情

EQUATION

反应方程式

HRID 443708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 14.7 g (0.0356 mol) of dimethyl 3-(α,α,α,α',α',α'-hexafluoro-3,5-xylyl)-4,5-isothiazoledicarboxylate, 7.2 g (0.18 mol) of NaOH, and 45 ml of water was held at reflux for 2 hours, was cooled, extracted twice with ether, and acidified with 30 ml (0.36 mol) of concentrated HCl. The resultant mixture was extracted three times with ether; these ether extracts were combined, dried (CaSO4), and concentrated under vacuum to 12.8 g (93.4%) of white solid, m.p. 193°-193.5° with decomposition.

WORKUP

后处理

  1. temperatureat reflux for 2 hours
  2. temperaturewas cooled
  3. extractionextracted twice with ether
  4. extractionThe resultant mixture was extracted three times with ether
  5. dry with materialdried (CaSO4)
  6. concentrationconcentrated under vacuum to 12.8 g (93.4%) of white solid, m.p. 193°-193.5° with decomposition