反应详情

温度

50 °C

To a solution of 4-chloro-2-fluoro-5-methoxybenzaldehyde (0.821 g, 4.35 mmol) in 8.7 mL of DMSO were successively added K2CO3 (1.81 g, 3 eq.) and methyl thioglycolate (0.474 mL, 1.2 eq.), and the mixture was vigorously stirred at 50° C. for 2 h. After cooling, the reaction mixture was poured onto crashed ice/HCl, twofold extracted with AcOEt, washed with water, dried over sodium sulfate, and evaporated. Flash chromatography (SiO2, hexane/AcOEt=85/15), followed by crystallization from heptane/AcOEt, yielded 0.300 g of the title compound as off-white solid.

1. temperatureAfter cooling
2. additionthe reaction mixture was poured
3. extractiontwofold extracted with AcOEt
4. washwashed with water
5. dry with materialdried over sodium sulfate
6. customevaporated
7. customFlash chromatography (SiO2, hexane/AcOEt=85/15), followed by crystallization from heptane/AcOEt