HRID1753222

反应详情

EQUATION

反应方程式

HRID 1753222 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of ethyl 6-(dimethylamino)-5-methylpyrimidine-4-carboxylate (45) (60.0 g, 287.0 mmol) in EtOH (600 mL) was added in portionwise NaBH4 (21.82 g, 574.0 mmol) at 0° C. and the mixture was stirred for 16 h at RT. The solvent was evaporated under the reduced pressure and the reaction mixture was poured in to water (200 mL) and extracted with ethyl acetate (3×100 mL). The combined organic layer was washed with water, brine, dried over sodium sulfate and concentrated at reduced pressure to yield (6-(dimethylamino)-5-methylpyrimidin-4-yl)methanol (46); 47 g, (97%).

WORKUP

后处理

  1. customThe solvent was evaporated under the reduced pressure
  2. additionthe reaction mixture was poured in to water (200 mL)
  3. extractionextracted with ethyl acetate (3×100 mL)
  4. washThe combined organic layer was washed with water, brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated at reduced pressure