HRID2386014

反应详情

EQUATION

反应方程式

HRID 2386014 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 49 mg (0.12 mmol) of 1-(8-Bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepin-2-yl)-5,5-dimethylimidazolidin-2,4-dione from Example 485, and 0.0334 ml (0.24 mmol) of triethylamine in 5 ml of ethanol was hydrogenated over 120 mg of 10% palladium on charcoal at 1 atm for 3 hours. The mixture was filtered through celite and concentrated in vacuum. The residue was purified on 4 g siligal column eluting the product with ethyl acetate gradient in heptane to give 493. Yield 20 mg (51%). MS (ESI+): 330.1

WORKUP

后处理

  1. filtrationThe mixture was filtered through celite and
  2. concentrationconcentrated in vacuum
  3. customThe residue was purified on 4 g siligal column
  4. washeluting the product with ethyl acetate gradient in heptane