反应详情

To a solution of 2,5-dimethoxytoluene (4.66 g, 30.6 mmol) in 60 mL of N-methyl-N-phenyl-formamide was added at 0° C. POCl3 (8.41 mL, 3 eq.), and the mixture was heated for 60 Min. to 80° C. After cooling, the reaction mixture was poured onto crashed ice, twofold extracted with AcOEt, washed with water, dried over sodium sulfate, and evaporated to dryness. Flash chromatography (SiO2, hexane/AcOEt=9/1) afforded 4.153 g of the title compound as off-white solid.

1. customto 80° C
2. temperatureAfter cooling
3. additionthe reaction mixture was poured
4. extractiontwofold extracted with AcOEt
5. washwashed with water
6. dry with materialdried over sodium sulfate
7. customevaporated to dryness