反应详情

温度

23 °C

A mixture of (+)-2-Fluoro-4(2-methylbutyl)biphenyl (10 gram) and trans-4-n-butylcyclohexylacetyl chloride (9.4 gram) in dichloromethane (20 ml) was added over 20 minutes to a cooled (5°-10° C.), stirred suspension of anhydrous aluminium chloride 6.1 gram) in dichloromethane (20 ml). After the addition the reaction mixture was allowed to warm to 23° C. and left stirring for 17 hours. The resulting solution was added to water (200 ml), extracted successively with petroleum spirit (bp. 60°-80°:180 ml +100 ml). The organic extract was then washed with water (200 ml), dried over anhydrous sodium sulphate (5 gram) and evaporated. The yellow crystalline residue (17.9 gram) was recrystallised from ethanol (35 ml) at 25° C. to give the product (14.8 gram; 85% yield). The product had mp=71.4°-72.1° C.; VirtualCH-I, (68.5°-68.8° C.). It was found to be 99.5 % pure by glc.

1. additionwas added over 20 minutes to
2. temperaturea cooled (5°-10° C.)
3. additionAfter the addition the reaction mixture
4. waitleft
5. stirringstirring for 17 hours
6. extractionextracted successively with petroleum spirit (bp. 60°-80°:180 ml +100 ml)
7. extractionThe organic extract
8. washwas then washed with water (200 ml)
9. dry with materialdried over anhydrous sodium sulphate (5 gram)
10. customevaporated
11. customThe yellow crystalline residue (17.9 gram) was recrystallised from ethanol (35 ml) at 25° C.
12. customto give the product (14.8 gram; 85% yield)
13. customVirtualCH-I, (68.5°-68.8° C.)