反应详情

In a 2 liter, 4 neck round bottom flask equipped with a mechanical stirrer, a solution of 75 grams of 1,4-butanediol, 240 grams of chloroacetic acid and 3 grams of para-toluenesulphonic acid 750 ml toluene was refluxed for 6 hours using a Dean-Stark apparatus. The solution was then cooled to room temperature. The toluene layer was washed with water (2×300 ml), 5% sodium bicarbonate solution (3×500 ml), water (2×300 ml), dried over sodium sulfate, and distilled to get crude 21, which was purified by recrystallization in chloroform:hexane (1:7) to get 92 grams of pure 21 as a white fluffy powder. m.p: 74-76.5° C., 1H NMR (CDCl3) δ 1.78 (t, 2H, CH2), 4.05 (s, 2H, CH2), 4.25 (t, 2H, CH2)

1. customIn a 2 liter, 4 neck round bottom flask equipped with a mechanical stirrer
2. washThe toluene layer was washed with water (2×300 ml), 5% sodium bicarbonate solution (3×500 ml), water (2×300 ml)
3. dry with materialdried over sodium sulfate
4. distillationdistilled
5. customto get crude 21, which
6. customwas purified by recrystallization in chloroform:hexane (1:7)
7. customto get 92 grams of pure 21 as a white fluffy powder