HRID910857

反应详情

EQUATION

反应方程式

HRID 910857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The subtitle compound was prepared by using the product from step i). (3.48 g) was added to a solution of triethylamine (10 ml) and formic acid (7 ml) in DMF (30 ml) after 20 minutes. Meldrum's acid (3.22 g) was added and the mixture heated to 100 C for 4 hours. The solution was basified with 2M NaOH, extracted with ether (discarded). The aqueous layer was acidified with 2M HCl, extracted with ethyl acetate, dried and concentrated under reduced pressure to give an oil. The residue was purified by chromatography on silica eluting with diethyl ether/isohexane 1:5, yield 0.40 g.

WORKUP

后处理

  1. temperaturethe mixture heated to 100 C for 4 hours
  2. extractionextracted with ether (discarded)
  3. extractionextracted with ethyl acetate
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customto give an oil
  7. customThe residue was purified by chromatography on silica eluting with diethyl ether/isohexane 1:5, yield 0.40 g