反应详情

Phosphorus oxychloride (1.15 mL; 15.4 mM) was added slowly to stirring dimethylformamide (0.95 mL; 12.2 mM) at -10° under nitrogen. The resulting mixture was stirred for 15 mins. 2-(3'-bromophenyl)thiophene (2.12 g; 9 mM) was then added. The reaction mixture was then warmed slowly to 110° over a period of 1 hr. cooled and poured into ice, and cautiously neutralized with sodium carbonate. Extraction with ethyl acetate and drying the organic phase with anhydrous magnesium sulfate provided upon concentration 2.16 g of the desired aldehyde as an oily solid.

1. temperatureThe reaction mixture was then warmed slowly to 110° over a period of 1 hr
2. temperaturecooled
3. additionpoured into ice
4. extractionExtraction with ethyl acetate
5. dry with materialdrying the organic phase with anhydrous magnesium sulfate