HRID2072953
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
Solid N-[3-[(3-chlorobenzoyl)amino]-2-pyridinyl]glycine ethyl ester, 12.84 g (0.038 mole) was heated in glass at 210°-20° C. in a Wood's metal bath for 7 minutes. The residue was dissolved in methylene chloride, treated with charcoal, and filtered through a Celite pad. The orange filtrate was treated with Florisil® to give a pink filtrate. The filtrate was evaporated to give a solid, which was recrystallized from tetrahydrofuran-petroleum ether. The solid was collected, washed with petroleum ether, and dried under high vacuum at 50° C. for 5 hours to give 5.3 g (44%) of title compound, mp 98°-99.8° C.
WORKUP
后处理
- filtrationfiltered through a Celite pad
- additionThe orange filtrate was treated with Florisil®
- customto give a pink filtrate
- customThe filtrate was evaporated
- customto give a solid, which
- customwas recrystallized from tetrahydrofuran-petroleum ether
- customThe solid was collected
- washwashed with petroleum ether
- customdried under high vacuum at 50° C. for 5 hours