反应详情

A mixture of 9500 ml of anhydrous ethyl alcohol and 2323 g of 1-(4-aminocyclohexyl)-2-imidazolidinone is heated with mixing to effect solution. The solution is cooled to room temperaure and 3200 ml of a saturated solution of anhydrous hydrogen chloride gas in ethyl acetate is added to pH 1. The temperature of the mixture rises to 60° and the product crystallizes. The mixture is cooled to 10°. The crude product is filtered off, washed with 3500 ml of anhydrous ethyl alcohol and dried at 50°-60° in vacuo for 2 days. The crude hydrochloride salt is recrystallized twice from anhydrous methanol-ethyl ether (ca 1:1) to give cis 1-(4-aminocyclohexyl)-2-imidazolidinone monohydrochloride, m.p. 327°-8°.

1. temperatureis heated
2. additionwith mixing
3. additionis added to pH 1
4. customrises to 60°
5. customthe product crystallizes
6. temperatureThe mixture is cooled to 10°
7. filtrationThe crude product is filtered off
8. washwashed with 3500 ml of anhydrous ethyl alcohol
9. customdried at 50°-60° in vacuo for 2 days
10. customThe crude hydrochloride salt is recrystallized twice from anhydrous methanol-ethyl ether (ca 1:1)