HRID1827764

反应详情

EQUATION

反应方程式

HRID 1827764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.5 g (2.8 mmol) of 6-benzyloxy-8-{2-[2-(4-ethoxyphenyl)-1,1-dimethylethylamino]-1-hydroxyethyl}4H-benzo[1,4]oxazin-3-one in 80 mL methanol are hydrogenated with 250 mg palladium on charcoal (10%) as catalyst at ambient temperature and normal pressure. The catalyst is suction filtered and the filtrate is evaporated down. The residue is dissolved in 5 mL ethanol by heating, seeded, and diluted with ethyl acetate. The solid precipitated is filtered off and washed. White solid. Yield 1.0 g (83%, hydrochloride); melting point: 232° C.–235° C.; mass spectrometry: [M+H]+=401.

WORKUP

后处理

  1. filtrationfiltered
  2. customthe filtrate is evaporated down
  3. dissolutionThe residue is dissolved in 5 mL ethanol
  4. temperatureby heating
  5. additiondiluted with ethyl acetate
  6. customThe solid precipitated
  7. filtrationis filtered off
  8. washwashed