反应详情

n-Butyl glycolate (231 g; 1.75 mol) and imidazole (345.1 g; 5.07 mol) are placed together at 0° C. The suspension obtained was treated portionwise with t-butyldimethylchlorosilane (303 g; 2.01 mol) during 1.5 hours. After 20 hours at room temperature the reaction mixture was diluted with ether/n-hexane 1:1 (1 l) and suction filtered. The crystals were rinsed thoroughly with ether/n-hexane 1:1 (200 ml). The filtrate was washed in succession with water (2×700 ml) and saturated aqueous sodium chloride solution (500 ml), dried over magnesium sulphate and concentrated. The oil obtained was distilled over a Vigreux column (7.5 cm). Yield: 405 g (94%) as a colourless oil (b.p. 78° C./0.98 mmHg).

1. customare placed together at 0° C
2. customThe suspension obtained
3. filtrationfiltered
4. washThe crystals were rinsed thoroughly with ether/n-hexane 1:1 (200 ml)
5. washThe filtrate was washed in succession with water (2×700 ml) and saturated aqueous sodium chloride solution (500 ml)
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated
8. customThe oil obtained
9. distillationwas distilled over a Vigreux column (7.5 cm)