HRID222565

反应详情

EQUATION

反应方程式

HRID 222565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of tert-butyldiphenylsilyl chloride (20.32 g, 74.03 mmol) and imidazole (6.25 g, 91.9 mmol) was treated dropwise with 2-bromoethanol (47, 5 mL, 8.87 g, 70.8 mmol). Stirring was continued for 12 h. The mixture was diluted with Et2O and water. The phases were separated, and the aqueous layer was extracted Et2O. The organic extract was washed with water and dried over Na2SO4. Concentration of the sample yielded a pale brown oil (26.01 g, 97%): 1H NMR δ 1.11 (s, 9H), 3.45 (t, J=6.3 Hz, 2H), 3.96 (t, J=6.3 Hz, 2H), 7.42-7.47 (m, 6H), 7.70-7.73 (m, 4H); 13C NMR δ 19.52, 27.03, 33.43, 64.24, 128.04, 130.10, 133.49, 135.84.

WORKUP

后处理

  1. customThe phases were separated
  2. extractionthe aqueous layer was extracted Et2O
  3. extractionThe organic extract
  4. washwas washed with water
  5. dry with materialdried over Na2SO4