反应详情

温度

0 °C

Ethyl 2-hydroxy-2-(thiophen-2-yl)acetate (I26) (4.58 g, 24.6 mmol) was dissolved in dry DCM (125 ml) and cooled at 0° C. DIPEA (5.15 ml, 29.5 mmol) and methanesulphonyl chloride (2.11 ml, 27.1 mmol) were added, and the resulting solution was stirred at room temperature for 1 hour. DIPEA (0.86 ml, 4.92 mmol) and methanesulphonyl chloride (0.19 ml, 2.46 mmol) were added again. After 1 additional hour, a third portion of DIPEA (0.43 ml, 2.46 mmol) and methanesulphonyl chloride (77 ul, 0.98 mmol) was added. After 1 hour, the reaction was completed. The mixture was diluted with DCM, washed with sat. NaHCO3, water and brine, dried (Na2SO4), filtered, and evaporated. The resulting oil was used for the next step without any further purification.

1. waitAfter 1 hour
2. washwashed with sat. NaHCO3, water and brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customThe resulting oil was used for the next step without any further purification