HRID367362

反应详情

EQUATION

反应方程式

HRID 367362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 500 mL RBF equipped with a mechanical stirrer was charged with AlCl3 (35.4 g) and CHCl3 (300 mL) and cooled in an ice bath. Then 2-methylbutanoyl chloride (31.4 g) was added over 0.5 h to the ice-cold suspension. Keeping the internal temperature <10° C., thioanisole (31.2 mL) was added dropwise over 1 h. After completion of addition, the resulting mixture was stirred at r.t. for 2 h. The resulting suspension was poured onto an ice-water mixture and stirred until decoloraton. The organic layer was separated, washed with water, dried over Na2SO4 and concentrated to dryness. The resulting white solid was swished in hexane and collected by filtration to give the title compound as a white solid. 1H NMR(CD3COCD3): δ0.88 (3H, t), 1.12 (3H, d), 1.47 (1H, m), 1.78 (1H, m), 2.57 (3H, s), 3.49 (1H, m), 7.37 (2H, d), 7.93 (2H, d).

WORKUP

后处理

  1. customA 500 mL RBF equipped with a mechanical stirrer
  2. temperaturecooled in an ice bath
  3. additionwas added dropwise over 1 h
  4. additionAfter completion of addition
  5. stirringstirred until decoloraton
  6. customThe organic layer was separated
  7. washwashed with water
  8. dry with materialdried over Na2SO4
  9. concentrationconcentrated to dryness
  10. filtrationcollected by filtration