HRID1528167

反应详情

EQUATION

反应方程式

HRID 1528167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of methylamine (2 M in methanol) at 0° C. was added dropwise to a solution of 14.82 g of ethyl 2-bromomethyl-6-methoxybenzoate in methanol and the reaction medium was stirred for 5 hours at 0° C. and left to stir at ambient temperature for 2 days. The solvent was evaporated off and 30 ml of a saturated sodium hydrogen carbonate solution were added to the residue. The product was extracted with ethyl acetate (3×50 ml). The organic phases were combined, dried over magnesium sulfate and evaporated. The residue was purified by chromatography on silica gel. 4.52 g of 7-methoxy-2-methyl-2,3-dihydroisoindol-1-one were obtained. Yield=47%.

WORKUP

后处理

  1. waitleft
  2. stirringto stir at ambient temperature for 2 days
  3. customThe solvent was evaporated off
  4. addition30 ml of a saturated sodium hydrogen carbonate solution were added to the residue
  5. extractionThe product was extracted with ethyl acetate (3×50 ml)
  6. dry with materialdried over magnesium sulfate
  7. customevaporated
  8. customThe residue was purified by chromatography on silica gel