反应详情

温度

0 °C

Saturate a suspension of anhydrous stannous chloride (378 mg; 2 mmole) in 7.5 ml dry ether with hydrogen chloride at a temperature of 0°-5° C., and add 235 mg (1 mmole) of 3-cyano-dibenzo[b,f]thiepin. Stir for one hour at 0° C. and allow to warm to room temperature (25° C.). Continue stirring at room temperature for approximately 48 hours. Add 5 ml of water and 1 ml 2N hydrochloric acid, and extract with a mixture of 5 ml ether and 5 ml ethyl acetate. When the hydrolysis of the chloro stannate is complete, evidenced by the disappearance of solids from the solution, separate the organic layer containing the product, wash with water/sodium chloride solution, and after drying, evaporate the solution to produce a dark oil which solidifies when triturated with hexane. The title product is obtained when the above solid material is crystallized from acetonitrile, m.p. 114.5°-115.5° C.

1. concentrationSaturate
2. temperatureto warm to room temperature (25° C.)
3. stirringContinue stirring at room temperature for approximately 48 hours
4. extractionextract with a mixture of 5 ml ether and 5 ml ethyl acetate
5. customWhen the hydrolysis of the chloro stannate
6. customseparate the organic layer
7. additioncontaining the product
8. washwash with water/sodium chloride solution
9. customafter drying
10. customevaporate the solution
11. customto produce a dark oil which
12. customtriturated with hexane