HRID1277613

反应详情

EQUATION

反应方程式

HRID 1277613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 25.37 g. (0.143 mol.) of methyl 2-carboxyethyldithiocarbamate and 5.6 g. (0.143 mol.) of sodium hydroxide in 210 ml. of water was added 9.25 g. (0.143 mol.) of sodium azide. The reaction mixture was refluxed for one hour then cooled, diluted with 100 ml. of ether and acidified to pH 1.7. The layers were separated, the aqueous phase was extracted with ether and the combined extracts were dried (MgSO4) and evaporated to dryness to give a residue which was recrystallized from acetone-chloroform to give 1-(2-carboxyethyl)tetrazole-5-thiol, m.p. 158°-160° C.

WORKUP

后处理

  1. additionTo a mixture of 25.37 g
  2. temperatureThe reaction mixture was refluxed for one hour
  3. temperaturethen cooled
  4. additiondiluted with 100 ml
  5. customThe layers were separated
  6. extractionthe aqueous phase was extracted with ether
  7. dry with materialthe combined extracts were dried (MgSO4)
  8. customevaporated to dryness
  9. customto give a residue which
  10. customwas recrystallized from acetone-chloroform