反应 #355758

反应方程式

phenothiazine

iodoethane

potassium hydroxide

→

10-Ethylphenothiazine

溶剂

toluene

反应条件

后处理

1. 1
   温度was refluxed for 24 hours
2. 2
   温度After cooling
3. 3
   过滤the reaction mixture was filtered
4. 4
   其他the solvent was evaporated
5. 5
   其他The product was recrystallized from methanol
6. 6
   其他was 103-104° C

实验过程

A mixture of 10 g (0.05 mol) of phenothiazine (obtained from Fluka), 11.7 g (0.075 mol) of iodoethane (obtained from Aldrich), 4.2 g (0.075 mol) of potassium hydroxide and 0.25 g of tetra-n-butylammonium hydrogen sulfate (obtained from Aldrich) in 200 ml of dry toluene was refluxed for 24 hours. After cooling, the reaction mixture was filtered and the solvent was evaporated. The product was recrystallized from methanol. The yield of 10-ethylphenothiazine (C14H13NS, FW=227.33) was 90%. The melting point of the product was 103-104° C. The 1H-NMR spectrum (100 MHz) of the product in CDCl3 was characterized by the following chemical shifts (δ, ppm): 1.40 (t, J=7.0 Hz, 3H, CH3); 3.90 (q, J=7.0 Hz, 2H, CH2); 6.78-7.32 (m, 8H, Ar).

来源