HRID1154316

反应详情

EQUATION

反应方程式

HRID 1154316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-isopropenyl pyridine (1.79 g) and isothiazolidine-1,1-dioxide (1.81 g) was heated at 130° C. during the addition of "Triton B" (Trade Mark, trimethylbenzylammonium hydroxide) (0.25 g added every hour for four hours; 40% solution in water). After stirring for 16 hours at 130° the mixture was cooled and taken in chloroform (50 cm3) and water (50 cm3). The aqueous phase was extracted with chloroform (3×20 cm3) and the dried (MgSO4) extracts were evaporated to given an oil. Chromatography on silica ("Merck 60. 9385") eluting with ethyl acetate gave 2-[2-(4-pyridyl)prop-1-yl]isothiazolidine-1,1-dioxide which crystallised from ethyl acetate-hexane as needles, m.p. 90°-92° (1.01 g).

WORKUP

后处理

  1. additionadded every hour for four hours
  2. temperaturewas cooled
  3. extractionThe aqueous phase was extracted with chloroform (3×20 cm3)
  4. dry with materialthe dried (MgSO4) extracts
  5. customwere evaporated
  6. washChromatography on silica ("Merck 60. 9385") eluting with ethyl acetate