HRID467777

反应详情

EQUATION

反应方程式

HRID 467777 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 3-(bis(tert-butoxycarbonyl)amino)-6-bromopyrazine-2-carboxylate (500 mg, 1.16 mmol; example A-10, step 1) in MeOH (10 ml) was added sodium methoxide (30%; 280 μl, 1.5 mmol) at room temperature and stirring was continued at r.t. for 2 h. The reaction mixture was poured into ethyl acetate (75 ml) and extracted with potassium hydrogen sulfate (10%). The organic phase was washed with water and brine and the aqueous layers were back-extracted with ethyl acetate. The organic layers were dried and evaporated and the product was obtained after purification by silica gel chromatography using a heptane/ethyl acetate gradient as colorless solid (320 mg, 71%).

WORKUP

后处理

  1. customat room temperature
  2. extractionextracted with potassium hydrogen sulfate (10%)
  3. washThe organic phase was washed with water and brine
  4. extractionthe aqueous layers were back-extracted with ethyl acetate
  5. customThe organic layers were dried
  6. customevaporated
  7. customthe product was obtained
  8. customafter purification by silica gel chromatography