反应详情

To a solution of morpholine (89.3 mmoles) in acetic acid (50 ml) at 0° C. there are added 1-(1H-pyrrol-2-yl)-propan-1-one (81.2 mmoles) and formaldehyde (89.3 mmoles) 37% in water. The reaction mixture is stirred overnight at ambient temperature. After concentration of the mixture, the solution is brought to alkaline pH (10-12) using 20% aqueous NaOH solution at 0° C. and is then extracted with DCM. The organic phase is washed with water and with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness and purified by flash chromatography on silica gel (SiO2; gradient 100% AcOEt to AcOEt/MeOH 9/1) to yield the title product.

1. customat 0° C.
2. extractionis then extracted with DCM
3. washThe organic phase is washed with water and with saturated aqueous NaCl solution
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. customevaporated to dryness
7. custompurified by flash chromatography on silica gel (SiO2; gradient 100% AcOEt to AcOEt/MeOH 9/1)