HRID1189398

反应详情

EQUATION

反应方程式

HRID 1189398 的结构方程式

PROCEDURE

实验过程

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of [5-(2-methyl-[1,3]dioxolan-2-yl)-thiophen-2-yl]-acetonitrile (2.67 g, 12.77 mmol) in a 1:1 mixture of MeOH and H2O (11 mL) was treated at rt with KOH (1.43 g, 25.54 mmol). After stirring at reflux for 1.5 h, the cooled reaction mixture was washed with ether. The aq. phase was carefully acidified to pH 4-5 with 1M HCl and the product was extracted several times with CH2CL2. The combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a brown oil. LC-MS-conditions 02: tR=0.79 min.

WORKUP

后处理

  1. temperatureat reflux for 1.5 h
  2. customthe cooled reaction mixture
  3. washwas washed with ether
  4. extractionthe product was extracted several times with CH2CL2
  5. dry with materialextracts were dried over Na2SO4
  6. filtrationfiltered
  7. customthe solvents were removed under reduced pressure