HRID468553

反应详情

EQUATION

反应方程式

HRID 468553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Pd/C (100 mg) was added as a single portion to a degassed and flushed (3×Ar) suspension of 7-nitroquinazolin-4-one (1.15 g, 6.02 mmol) in methanol (150 mL). The resulting black mixture was degassed, flushed with hydrogen and allowed to stir for 4 hours. The mixture was filtered through celite, washed well with methanol, and the filtrate concentrated to give a tanned solid. This was purified by column chromatography (silica) using 10% methanol/ethyl acetate as the eluent. Combined fractions gave a beige solid (949 mg, 98% yield).

WORKUP

后处理

  1. customa degassed
  2. customflushed
  3. customThe resulting black mixture was degassed
  4. customflushed with hydrogen
  5. filtrationThe mixture was filtered through celite
  6. washwashed well with methanol
  7. concentrationthe filtrate concentrated
  8. customto give a tanned solid
  9. customThis was purified by column chromatography (silica)