HRID895056
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 hyroxide 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°.
WORKUP
后处理
- additionTo a mixture of 25.37 g
- temperatureThe reaction mixture was refluxed for one hour
- temperaturethen cooled
- additiondiluted with 100 ml
- customThe layers were separated
- extractionthe aqueous phase was extracted with ether
- dry with materialthe combined extracts were dried (MgSO4)
- customevaporated to dryness
- customto give a residue which
- customwas recrystallized from acetone-chloroform