反应详情

温度

0 °C

A slurry was prepared from 8.75 g. (0.05 mole) of N-acetyl-2-(acetylthio)acetamide and 100 ml. of methanol at -5° C., and nitrogen was bubbled through the slurry. There was then added 2.0 g. (0.05 mole) of sodium hydroxide in 20 ml. of methanol. The reaction mixture was aged for 1 hour and then concentrated under high vacuum while the temperature was kept below 30° C. Next, 100 ml. of dimethylformamide was added and the reaction mixture was cooled to 0° C. There was then added 7.2 g. (0.055 mole) of 2-furoyl chloride, and the reaction mixture was aged for 3 hours at 0° C., after which it was concentrated under high vacuum. The residue was charged to a silica gel column and eluted with 50% ethylacetate/hexane. The product was recrystallized from toluene and air dried to yield 2.9 g., m.p. 126°-128° C.

1. customA slurry was prepared from 8.75 g
2. customof methanol at -5° C., and nitrogen was bubbled through the slurry
3. additionThere was then added 2.0 g
4. concentrationconcentrated under high vacuum while the temperature
5. customwas kept below 30° C
6. additionof dimethylformamide was added
7. additionThere was then added 7.2 g
8. concentrationafter which it was concentrated under high vacuum
9. additionThe residue was charged to a silica gel column
10. washeluted with 50% ethylacetate/hexane
11. customThe product was recrystallized from toluene and air
12. customdried
13. customto yield 2.9 g