反应详情

A mixture of 2.00 g of trans-4-cyanocyclohexanecarboxaldehyde, 2.13 g of 2-pentyl-1,3-propanediol and 65 mg of p-toluenesulphonic acid in 100 ml of benzene was heated to reflux for 3 hours while gassing with argon and with separation of water in a round flask provided with a water separator and a reflux condenser. The mixture was subsequently treated with 3.0 g of potassium carbonate, stirred at room temperature for 16 hours, then filtered and the filtrate was concentrated. Recrystallization of the crystalline residue (4.1 g) from hexane at 0° C. gave 1.47 g (38%) of trans-4-(trans-5-pentyl-m-dioxan-2-yl)cyclohexanecarbonitrile as colourless crystals in a purity of 99.1%. After a further recrystallization from hexane at 0° C., the purity increased to 99.9%; m.p. (C--N) 45.6° C., cl.p. (N--I) 46.7° C.

1. temperaturewas heated
2. temperatureto reflux for 3 hours
3. customwhile gassing with argon and with separation of water in a round flask
4. customprovided with a water separator and a reflux condenser
5. filtrationfiltered
6. concentrationthe filtrate was concentrated
7. customRecrystallization of the crystalline residue (4.1 g) from hexane at 0° C.