HRID330293
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred, partial solution of NaCN (11.4 g, 0.232 mol) in DMSO 75 mL) was added 5-chloromethylindan (35.2 g, 0.211 mol) dropwise over 45 minutes. (The internal temperature was maintained below 65° C.). The resulting mixture was stirred at room temperature overnight. H2O (250 mL) was added and the mixture was extracted with ether. The organic phase was washed with H2O (200 mL), 6N HCl (100 mL), H2O (200 mL), saturated aqueous NaHCO3 (100 mL), and saturated aqueous NaCl, dried (MgSO4), and concentrated. The crude product was distilled under reduced pressure (0.6 mm) to give 28.1 g (85%) as a colorless oil, b.p. 131°) C.
WORKUP
后处理
- temperature(The internal temperature was maintained below 65° C.)
- extractionthe mixture was extracted with ether
- washThe organic phase was washed with H2O (200 mL), 6N HCl (100 mL), H2O (200 mL), saturated aqueous NaHCO3 (100 mL), and saturated aqueous NaCl
- dry with materialdried (MgSO4)
- concentrationconcentrated
- distillationThe crude product was distilled under reduced pressure (0.6 mm)
- customto give 28.1 g (85%) as a colorless oil, b.p. 131°) C