反应详情

温度

95 °C

A mixture of (R)-2,3-dihydrobenzo[1,4]dioxine-2-carboxylic acid (167 mg, 0.93 mmol), thionyl chloride (338 μl, 551 mg, 4.63 mmol) and dry toluene was heated at 95° C. for 1.5 h and then evaporated to dryness. Toluene was added and the evaporation was repeated. The evaporation residue was dissolved in DCM (2 ml) and added slowly to a cold solution (0° C.) of 3-benzo[1,3]dioxol-5-yl-piperidine HCl (224 mg, 0.93 mmol) and DIPEA (0.324 ml, 240 mg, 1.85 mmol) in DCM (5 ml). The reaction mixture was stirred for 1 h 45 min at RT. Water was added, layers were separated and the organic phase was washed twice with 1 M HCl and sat. NaHCO3. The organic phase was dried (Na2SO4), filtered and evaporated to give 290 mg of the title compound.

1. customevaporated to dryness
2. additionToluene was added
3. customthe evaporation
4. dissolutionThe evaporation residue was dissolved in DCM (2 ml)
5. customlayers were separated
6. washthe organic phase was washed twice with 1 M HCl and sat. NaHCO3
7. dry with materialThe organic phase was dried (Na2SO4)
8. filtrationfiltered
9. customevaporated