HRID621880

反应详情

EQUATION

反应方程式

HRID 621880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationfiltered through a Celite pad
  2. additionThe orange filtrate was treated with Florisil®
  3. customto give a pink filtrate
  4. customThe filtrate was evaporated
  5. customto give a solid, which
  6. customwas recrystallized from tetrahydrofuran-petroleum ether
  7. customThe solid was collected
  8. washwashed with petroleum ether
  9. customdried under high vacuum at 50° C. for 5 hours