反应详情

Thirty grams of 2-chlorodibenzo[b,f]oxepin-10(11H)-one, prepared in accordance with the procedure of Example 3, 45 grams of N-methylpiperazine and a solution of 8 grams of p-toluenesulfonic acid monohydrate in 150 ml of xylene are refluxed for a period of 22 hours in a reflux apparatus equipped with a Dean-Stark trap in order to remove the water that forms. The reaction mixture is cooled, treated with a solution of sodium bicarbonate, washed with water until the water washings are neutral, dried over anhydrous sodium sulfate and filtered through a column of neutral aluminum oxide. The filtrate is concentrated to dryness in vacuo and the residue, 46 grams, crystallized from ethanol to yield 32 grams of 1-(2-chlorodibenzo[b,f]oxepin-10-yl)-4-methylpiperazine having an m.p. of 119°-121° C.

1. customequipped with a Dean-Stark trap in order
2. customto remove the water that forms
3. temperatureThe reaction mixture is cooled
4. additiontreated with a solution of sodium bicarbonate
5. washwashed with water until the water washings
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered through a column of neutral aluminum oxide
8. concentrationThe filtrate is concentrated to dryness in vacuo
9. customthe residue, 46 grams, crystallized from ethanol