HRID267348

反应详情

EQUATION

反应方程式

HRID 267348 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 64.0 g. (0.28 mole) of methyl γ-iodobutyrate, 28.0 g. (0.28 mole) of triethylamine, 28.7 g. (0.28 mole) of thiomorpholine (J. Am. Chem. Soc. 76, 1187 (1954)) and 1 liter of benzene was stirred and heated at 60°-70°C. for 18 hours. After cooling the reaction mixture, the precipitated amine hydroiodide was removed by suction filtration. The benzene solution was evaporated to give a orange-red residue which was vacuum distilled (b.p. 84°-85°C. at 0.1 mm) to give 28.38 g. (50%) of the product as a colorless liquid.

WORKUP

后处理

  1. additionA mixture of 64.0 g
  2. temperatureheated at 60°-70°C. for 18 hours
  3. temperatureAfter cooling the reaction mixture
  4. customthe precipitated amine hydroiodide was removed by suction filtration
  5. customThe benzene solution was evaporated
  6. customto give a orange-red residue which
  7. distillationdistilled (b.p. 84°-85°C. at 0.1 mm)
  8. customto give 28.38 g