HRID325734

反应详情

EQUATION

反应方程式

HRID 325734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of sodium hydride (0.13 g) in dry sulpholane (10 ml) was treated with ethyl tetrazole-5-carboxylate (0.71 g), and the mixture stirred for 20 minutes at room temperature. Benzyl chloride (0.7 g) was then added, and the mixture was stirred at 60°-65° C. overnight. The mixture was then poured onto ice (25 g) and the resulting oil was separated off and dissolved in diethyl ether (35 ml). The aqueous layer was extracted with a further quantity of diethyl ether (10 ml) and the combined ether extracts were dried over magnesium sulphate. Removal of the ether under reduced pressure gave a mixture (1.36 g) of ethyl 1-benzyl-1H-tetrazole-5-carboxylate and ethyl 2-benzyl-2H-tetrazole-5-carboxylate, containing a little sulpholane.

WORKUP

后处理

  1. stirringthe mixture was stirred at 60°-65° C. overnight
  2. additionThe mixture was then poured onto ice (25 g)
  3. customthe resulting oil was separated off
  4. dissolutiondissolved in diethyl ether (35 ml)
  5. extractionThe aqueous layer was extracted with a further quantity of diethyl ether (10 ml)
  6. dry with materialthe combined ether extracts were dried over magnesium sulphate
  7. customRemoval of the ether under reduced pressure