HRID895054
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
1-Carboxymethyltetrazole-5-thiol and 1,1-carbonyldiimidazole were reacted as described in Example 4. To the reaction mixture was added tetrahydrofuran saturated with dry ammonia gas. The resulting suspension was stirred for 2.5 hours and the solid which formed was collected by filtration, washed with tetrahydrofuran and dissolved in methanol. Amberlite IR-120 ion-exchange resin (50 g.) was added and the suspension was stirred for 15 minutes. The resin was then removed and washed with absolute methanol. The methanol solution was concentrated to give a residue which was dissolved in ether and triturated with acetone to give 1-carbamoylmethyltetrazole-5-thiol, m.p. 200° (dec.).
WORKUP
后处理
- customthe solid which formed
- filtrationwas collected by filtration
- washwashed with tetrahydrofuran
- dissolutiondissolved in methanol
- additionAmberlite IR-120 ion-exchange resin (50 g.) was added
- stirringthe suspension was stirred for 15 minutes
- customThe resin was then removed
- washwashed with absolute methanol
- concentrationThe methanol solution was concentrated
- customto give a residue which
- customtriturated with acetone