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358733-61-6

1-(4-BENZHYDRYL-PIPERAZIN-1-YL)-2-CHLORO-ETHANONE synthesis

1synthesis methods
-

Yield:358733-61-6 95%

Reaction Conditions:

with triethylamine in dichloromethane at 5 - 20; for 18 h;

Steps:

62 Example 62: 1-(4-benzhydryl-piperazin-1-yl)-2-(8-methoxy-3,4-dihydro-1H-isoquinolin-2-yl)-ethanone; 1-(4-benzhydryl-piperazin-1-yl)-2-chloro-ethanone

A solution of 1-BENZHYDRYL-PIPERAZINE (Acros, 12293) (5. 05G, 20MMOL) and Et3N (2.22g, 22MMOL) in CH2CL2 (20 ML) was cooled to 5°C using an ice/H20 cooling. CHLOROACETYL chloride (Aldrich, 10,449-3) (2. 5g, 22MMOL) in CH2C12 (5ML) was added drop wise such that the temperature remained below 20°C. Once addition was complete, the reaction was stirred for for a further 18HRS at ambient temperature. Deionised H20 (50 mL) was added and stirring continued for a further lhr. The organic layer was separated, washed with brine (3 x 100 mL), dried (MgSO4) and concentrated in vacuo to afford 1- (4-BENZHYDRYL-PIPERAZIN-1-YL)-2-CHLORO-ETHANONE as a brown oil, which was used without further purification. Yield 6.8g (95%). HPLC retention time, 4. 22MIN. Mass spectrum (ES+) m/z 329 (M + H).

References:

WO2005/5392,2005,A1 Location in patent:Page 67