Benzene → Cyclohexyl phenyl ketone

温度

2 °C

A solution of cyclohexanecarbonyl chloride (9.1 ml) in CH2Cl2 (25 ml) was added slowly under nitrogen atmosphere at 0-4° C. to a stirred mixture of AlCl3 (9.1 g), CH2Cl2 (25 ml) and benzene (50 ml). The resulting mixture was stirred for 1 hour at 0-4° C. and 12 hours at the room temperature. The mixture was poured into ice-water (200 ml, contains 1 ml of concentrated HCl) and stirred for 5 minutes. The phases were separated and the aqueous phase was washed with CH2CO2 (2×20 ml). The organic phases were combined and extracted with water (2×20 ml), 2.5% NaOH solution (2×30 ml) and water (2×20 ml). The organic phase was dried over Na2SO4 and evaporated. Yield was 12.0 g.

1. stirringstirred for 5 minutes
2. customThe phases were separated
3. washthe aqueous phase was washed with CH2CO2 (2×20 ml)
4. extractionextracted with water (2×20 ml), 2.5% NaOH solution (2×30 ml) and water (2×20 ml)
5. dry with materialThe organic phase was dried over Na2SO4
6. customevaporated

ORDレコード

ord-02badd5f167345fb8edeafd29fdabb7c

出典データセット

uspto-grants-2002_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06362211B1