反应详情

温度

50 °C

A mixture of 1.76 g of 4-anilinopiperidine, 2 g of the compound obtained in step C of EXAMPLE 8 and 0.75 g of potassium carbonate in 10 ml of DMF is heated at 50° C. for 1 hour 30 minutes. The reaction mixture is poured into water and extracted with AcOEt, the organic phase is washed three times with water and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (96/4; v/v) as the eluent. The product obtained is taken up with 10 ml of acetic anhydride and the reaction mixture is stirred for 48 hours at RT. It is concentrated under vacuum, the residue is extracted with AcOEt, the organic phase is washed twice with 20% aqueous ammonia solution, twice with water and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The product obtained is taken up with a saturated solution of gaseous HCl in ether and the solvent is evaporated off under vacuum to give 1.4 g of the expected product after crystallization from AcOEt. M.p.=195° C.

1. extractionextracted with AcOEt
2. washthe organic phase is washed three times with water
3. dry with materialwith saturated NaCl solution and dried over MgSO4
4. customthe solvent is evaporated off under vacuum
5. customThe residue is chromatographed on silica H
6. customThe product obtained
7. concentrationIt is concentrated under vacuum
8. extractionthe residue is extracted with AcOEt
9. washthe organic phase is washed twice with 20% aqueous ammonia solution, twice with water and with saturated NaCl solution
10. dry with materialdried over MgSO4
11. customthe solvent is evaporated off under vacuum
12. customThe product obtained
13. customthe solvent is evaporated off under vacuum