HRID1617124

反应详情

EQUATION

反应方程式

HRID 1617124 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The product from step (v) (Ig) was dissolved in THF (30 mL) then acetic acid (0.239 g, 0.23 ml) and methyl 2-(3-formylphenyl)acetate (0.709 g) were added followed by MeOH (0.5 mL). The reaction mixture was stirred at rt for 72 h then sodium borohydride (0.1506 g) was added. After 2 h a further portion of sodium borohydride (0.0452 g) was added and the reaction mixture stirred for 16 h. A further portion of sodium borohydride (0.1506 g) was added and stirred for 2 h. The reaction mixture was poured into saturated sodium bicarbonate solution and extracted with EtOAc. The solvents were evaporated and the product was purified by chromatography eluting with DCM:MeOH 97:3 to 80:20 to give the title compound 0.5 g.

WORKUP

后处理

  1. stirringthe reaction mixture stirred for 16 h
  2. stirringstirred for 2 h
  3. extractionextracted with EtOAc
  4. customThe solvents were evaporated
  5. customthe product was purified by chromatography
  6. washeluting with DCM:MeOH 97:3 to 80:20