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 solution of 0.5 parts of sodium in 40 parts of absolute ethanol are added in the cold 5.4 parts of 1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one methanesulfonate. The whole is stirred until all solid enters solution. The solution is further stirred and refluxed for 2 hours. After cooling, the reaction mixture is filtered from some inorganic matter and the filtrate is evaporated. The residue is dissolved in 80 parts of methylbenzene, boiled with activated charcoal, filtered and the filtrate is evaporated again. The solid residue is washed with cold methylbenzene and crystallized from 16 parts of methylbenzene, yielding 2.6 parts of 3,4-dihydro-2H-[1,3]oxazino[3,2-a]benzimidazole; mp. 116.5°-118.5° C.
WORKUP
后处理
- stirringThe solution is further stirred
- temperaturerefluxed for 2 hours
- temperatureAfter cooling
- filtrationthe reaction mixture is filtered from some inorganic matter
- customthe filtrate is evaporated
- dissolutionThe residue is dissolved in 80 parts of methylbenzene
- filtrationfiltered
- customthe filtrate is evaporated again
- washThe solid residue is washed with cold methylbenzene
- customcrystallized from 16 parts of methylbenzene