HRID902622

反应详情

EQUATION

反应方程式

HRID 902622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of {3-[4-(t-butyidimethylsilyloxy)but-1-ynyl]phenyl}acetic acid methyl ester (700 mg, 2.1 mmol) in MeOH (15 ml) was treated with 5% Pd/C (100 mg) and hydrogen gas (1 atm) for 1 hr. The catalyst was filtered, and the solvent evaporated. The residue was dissolved in THF (1 ml), and treated with tetrabutyl ammonium fluoride (2 ml of a 1N solution in THF) for 2 hr. The reaction was diluted with water and extracted with diethyl ether. The organic extracts were washed with water, dried, evaporated, and the volatile organics removed by vacuum to give the title compound as an oil (300 mg, 64%). MS (ESI) 223.2 (M+H)+.

WORKUP

后处理

  1. filtrationThe catalyst was filtered
  2. customthe solvent evaporated
  3. dissolutionThe residue was dissolved in THF (1 ml)
  4. additiontreated with tetrabutyl ammonium fluoride (2 ml of a 1N solution in THF) for 2 hr
  5. additionThe reaction was diluted with water
  6. extractionextracted with diethyl ether
  7. washThe organic extracts were washed with water
  8. customdried
  9. customevaporated
  10. customthe volatile organics removed by vacuum