反应详情

温度

0 °C

Chloroacetyl chloride (4.5 ml, 56.6 mmol) is added dropwise to a solution of 1-o-tolylpiperazine (8.31 [lacuna], 47.2 mmol) and calcium carbonate (14.2 g, 142 mmol) in methyl ethyl ketone (100 ml) cooled to 0° C. The reaction mixture is stirred at this temperature for 1 h 30 and is then filtered through Celite. The Celite is rinsed several times with ethyl acetate and 3M sodium hydroxide solution. The two phases of the filtrate are then separated and the organic phase is dried over magnesium sulfate, filtered and concentrated to give the expected product in the form of a brown solid.

1. filtrationis then filtered through Celite
2. washThe Celite is rinsed several times with ethyl acetate and 3M sodium hydroxide solution
3. customThe two phases of the filtrate are then separated
4. dry with materialthe organic phase is dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated