反应详情

The base was freed from 3.5 g (10.4 mmole) of the hydrochloride of 2-[(3,4-dichlorophenyl)dimethylaminomethyl]cyclohexanone obtained according to stage 1 with 30 ml of water and 10 ml of ammonia solution (25 vol. %), extracted three times, each time with 30 ml of ether, and the combined organic extracts were dried over sodium sulfate, filtered, and concentrated by evaporation on a rotary evaporator without heating (500 to 10 mbar). 3.0 g (10.0 mmole) of this base were dissolved in 10 ml of tetrahydrofuran, added dropwise while cooling with an ice bath to 6.0 ml (12.0 mmole) of benzylmagnesium chloride (2 M solution in tetrahydrofuran), and stirred for 15 hours at RT. The reaction mixture was worked up by adding 15 ml of saturated ammonium chloride solution while cooling in an ice bath, and was extracted three times at RT, each time with 15 ml of ether. The combined organic extracts were dried over sodium sulfate, filtered, and concentrated by evaporation on a rotary evaporator (500 to 10 mbar). 3.05 g of crude base (77.9% of theory) were obtained, from which 2.88 g of 1-benzyl-2-[(3,4-dichlorophenyl)dimethylaminomethyl]cyclohexanol, hydrochloride (67.1% of theory) were obtained according to the procedure described in Example 1 (3rd Stage) with chlorotrimethylsilane/water in 2-butanone. The hydrochloride decomposes on heating above 200° C.

1. customobtained
2. extractionextracted three times
3. dry with materialeach time with 30 ml of ether, and the combined organic extracts were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by evaporation on a rotary evaporator
6. temperaturewithout heating (500 to 10 mbar)
7. additionadded dropwise
8. temperaturewhile cooling in an ice bath
9. extractionwas extracted three times at RT
10. dry with materialThe combined organic extracts were dried over sodium sulfate
11. filtrationfiltered
12. concentrationconcentrated by evaporation on a rotary evaporator (500 to 10 mbar)