反应详情

温度

20 °C

To a stirred solution of 10.0 g of 1-(1-benzenesulfonyl-1H-indol-2-yl)-allyl alcohol (32 mmol) in 100 ml of pyridine were added dropwise 5,6 ml benzoyl chloride (48 mmol) at 10° C. The mixture was stirred for an additional 1 h at 20° C. Most of the pyridine was distilled off, the residue was given in portions to 300 ml of ice water. The pH was adjusted to 2-3 with conc. HCl. The water was distilled off and the residue was dissolved in 100 ml of diethyl ether. After about 1 h the product crystallized. The suspension was stirred in an ice bath for 2 h, the solid was filtered off. The crude material was recrystallized from 90 ml methanol and dried 12 h at 35° C.

1. distillationMost of the pyridine was distilled off
2. distillationThe water was distilled off
3. dissolutionthe residue was dissolved in 100 ml of diethyl ether
4. customAfter about 1 h the product crystallized
5. stirringThe suspension was stirred in an ice bath for 2 h
6. filtrationthe solid was filtered off
7. customThe crude material was recrystallized from 90 ml methanol
8. customdried 12 h at 35° C.