HRID1850415

反应详情

EQUATION

反应方程式

HRID 1850415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-methylbenzylamine (766 mg, 3.16 mmol) and potassium carbonate (1.09 g, 7.90 mmol) were added to a solution of DMA (5 mL) containing 2-(iodomethyl)-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran (1.00 g, 3.16 mmol) synthesized in Reference Example 126, and the mixture was stirred under heated reflux for 4 hours. The reaction solution was cooled to room temperature, and water and ethyl acetate were added thereto to separate an organic layer. The organic layer was washed with water and saturated saline, and dried using anhydrous magnesium sulfate, followed by concentration under reduced pressure. The residue was purified by silica gel chromatography (hexane-ethyl acetate 99:1-93:7) to give 730 mg of the title compound (yield: 75%).

WORKUP

后处理

  1. customsynthesized in Reference Example 126
  2. temperatureunder heated
  3. temperaturereflux for 4 hours
  4. customto separate an organic layer
  5. washThe organic layer was washed with water and saturated saline
  6. customdried
  7. concentrationfollowed by concentration under reduced pressure
  8. customThe residue was purified by silica gel chromatography (hexane-ethyl acetate 99:1-93:7)