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.