HRID2412317

反应详情

EQUATION

反应方程式

HRID 2412317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Alternatively, glycine ethyl ester hydrochloride (35.7 g, 0.256 mole) was suspended in dry acetonitrile (300 ml) containing phosgene (50.7 g, 0.512 mole) and the reaction mixture was refluxed. A few drops of dry pyridine was added after 1 hr. of refluxing. Unreacted glycine ethyl ester hydrochloride was filtered off and dry toluene (300 ml) was added then acetonitrile was distilled off. The toluene solution was refluxed for 1 hr. to obtain glycine ethyl ester isocyanate (IR 2250 cm-1). This isocyanate was reacted, without further purification, with anhydrous methanol.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed
  2. temperatureof refluxing
  3. filtrationwas filtered off
  4. additiondry toluene (300 ml) was added
  5. distillationacetonitrile was distilled off
  6. temperatureThe toluene solution was refluxed for 1 hr