反应详情

温度

100 °C

A mixture of 5 g of the product of Step A, 5.4 g of α-(chloromethyl)-1,4-benzodioxin-2-methanol, 5.5 g of sodium carbonate, 4.2 g of potassium iodide and 100 ml of dimethylformamide was heated at 100° C under nitrogen for 24 hours and was then cooled and filtered. The filtrate was poured into ice and the gum formed was extracted with methylene chloride. The organic phase was washed, dried over calcium chloride and evaporated to dryness. The brown oily residue was chromatographed over silica gel and was eluted with a 98-2 methylene chloride-methanol mixture. The combined eluates were evaporated to dryness and the residue was crystallized from isopropanol to obtain 2.5 g of α-(2,3-dihydro-1,4-benzodioxin-2-yl)-4-([1H]-indol-3-yl)-1,2,3,6-tetrahydro-1-pyridine-ethanol melting at 177° C.

1. temperaturewas then cooled
2. filtrationfiltered
3. additionThe filtrate was poured into ice
4. customthe gum formed
5. extractionwas extracted with methylene chloride
6. washThe organic phase was washed
7. dry with materialdried over calcium chloride
8. customevaporated to dryness
9. customThe brown oily residue was chromatographed over silica gel
10. washwas eluted with a 98-2 methylene chloride-methanol mixture
11. customThe combined eluates were evaporated to dryness
12. customthe residue was crystallized from isopropanol