HRID1646611

反应详情

EQUATION

反应方程式

HRID 1646611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

3.89 g of (RS) 1-hydroxy-4-indanecarbonitrile in 39 ml of pyridine is cooled to 0° C., 3.45 ml of acetic anhydride is added drop by drop, and the whole is agitated for 16 hours at 20° C. The reaction mixture is poured into 300 ml of water containing sodium chloride and extracted with isopropyl ether; the ethereal phase is washed with 2N hydrochloric acid and then with water until pH 7 is obtained. The ethereal phase is dried and brought to dryness, and the residue is taken up in 1,2-dichloroethane, and again concentrated to dryness under reduced pressure. The residue is taken up in 40 ml of hexane, agitated for one hour, filtered, and 4.46 g of expected product is recovered. M.p.=65° C.

WORKUP

后处理

  1. extractionextracted with isopropyl ether
  2. washthe ethereal phase is washed with 2N hydrochloric acid
  3. customwith water until pH 7 is obtained
  4. customThe ethereal phase is dried
  5. concentrationagain concentrated to dryness under reduced pressure
  6. stirringagitated for one hour
  7. filtrationfiltered
  8. custom4.46 g of expected product is recovered