反应详情

To a solution of 3,3-dimethyl-7-chloroheptanoic acid (428 g., 2.21 moles) in 3 l. of chloroform containing 3 ml. of N,N-dimethylformamide is added 500 ml. of thionyl chloride and the resulting solution is tested under reflux for three hours. The reaction solution then is concentrated in vacuo and the residual acid chloride is dissolved in a minimum amount of benzene and added slowly to a solution containing 1260 ml. of 95% ethanol and 2520 ml. of benzene and 390 ml. of collidine. After heating under reflux for one hour, the solution is concentrated and the residue is dissolved in ether washed with water, dilute sodium bicarbonate solution and saline solution, dried over magnesium sulfate and concentrated to give 415 g. of crude oil, which is distilled under vacuum to yield two fractions: 46.6 g. boiling at 75° C. (0.3 mm.) and 236.7 g. boiling at 75° C.-80° C. (0.3 mm). The total yield is 283.3 g. (60%) and the product is indicated to be 95% pure by g.l.c.

1. temperatureunder reflux for three hours
2. concentrationThe reaction solution then is concentrated in vacuo
3. dissolutionthe residual acid chloride is dissolved in a minimum amount of benzene
4. additionadded slowly to a solution
5. additioncontaining 1260 ml
6. temperatureAfter heating
7. temperatureunder reflux for one hour
8. concentrationthe solution is concentrated
9. dissolutionthe residue is dissolved in ether
10. washwashed with water, dilute sodium bicarbonate solution and saline solution
11. dry with materialdried over magnesium sulfate
12. concentrationconcentrated
13. customto give 415 g
14. distillationof crude oil, which is distilled under vacuum
15. customto yield two fractions