HRID581055

反应详情

EQUATION

反应方程式

HRID 581055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.15 g (16.7 mmol) of 2-chloro-6-hydroxy-benzothiazole are dissolved in 50 ml of dimethylformamide and after the addition of 5.68 g (33 mmol) of 2-diethylamino-ethyl chloride-hydrochloride and 8.3 g (60 mmol) of potassium carbonate the mixture was stirred for 20 hours at ambient temperature. It was then added to water and extracted with ethyl acetate. The extracts are dried and evaporated down. The evaporation residue is purified by column chromatography on neutral aluminium oxide (eluant: petroleum ether/ethyl acetate=6:1). Yield: 3.9 g (81.7% of theory), oil, 1H-NMR spectrum (200 MHz, CDCl3, signals at ppm): 1.08 (t, 6H); 2.65 (q, 4H); 2.9 (t, 2H); 4.09 (t, 2H); 7.08 (dd, 1H); 7.24 (d, 1H); 7.8 (d, 1H).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customThe extracts are dried
  3. customevaporated down
  4. customThe evaporation residue is purified by column chromatography on neutral aluminium oxide (eluant: petroleum ether/ethyl acetate=6:1)