HRID355660

反应详情

EQUATION

反应方程式

HRID 355660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 2-indanol (Aldrich) (105 g, 0.78 mol) in pyridine (16 mL, 0.2 mol) and 340 mL of chloroform at -15° C. was added PBr3 (84 mL, 0.89 mol) over 45 min. The reaction mixture was stirred overnight at room temperature and extracted by addition of 450 mL of chloroform and 500 g of ice. The organic layer was washed twice with water, and dried over Na2SO4. The solvent was evaporated in vacuo, leaving a brown semi-solid. The product was distilled rapidly in vacuo and then fractionated to give 69 g (45%) 2-bromoindane, bp 90°-93°/3 mmHg; nD23 =1.5837.

WORKUP

后处理

  1. extractionextracted by addition of 450 mL of chloroform and 500 g of ice
  2. washThe organic layer was washed twice with water
  3. dry with materialdried over Na2SO4
  4. customThe solvent was evaporated in vacuo
  5. customleaving a brown semi-solid
  6. distillationThe product was distilled rapidly in vacuo