反应详情

A mixture of 4-chlorobutyryl chloride (93 g, 0.66 mol), N,N-dimethylaniline (80 g, 0.66 mol) and tert-butanol (0.66 mol) in ethyl ether (100 mL) was refluxed for 5 h. The reaction was cooled, diluted with ether and washed with water, 10% citric acid, saturated NaCl and dried over Na2SO4. Crude product obtained after evaporation of the solvent was distilled under vacuum (10 mmHg). Pure product (79 g, 67%) boiling at 57-58° C. was collected. 1H NMR (DMSO-d6) δ 3.64 (t, J=7 Hz, 2H), 2.35 (t, J=7 Hz, 2H), 1.93 (q, 2H), 1.41 (s, 9H).

1. temperaturewas refluxed for 5 h
2. temperatureThe reaction was cooled
3. washwashed with water, 10% citric acid, saturated NaCl
4. dry with materialdried over Na2SO4
5. customCrude product obtained
6. customafter evaporation of the solvent
7. distillationwas distilled under vacuum (10 mmHg)
8. customPure product (79 g, 67%) boiling at 57-58° C. was collected