反应详情

To a solution of morpholine (98.5 mmoles) in acetic acid (100 ml) at 0° C. there are added 1-triisopropylsilanyl-1H-pyrrole (89.5 mmoles) and formaldehyde (89.5 mmoles) 37% in water. The reaction mixture is stirred overnight at ambient temperature. The solution is brought to alkaline pH (10-12) using 20% aqueous NaOH solution 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. The residue obtained is purified by flash chromatography on silica gel (SiO2; gradient DCM/AcOEt) to yield the title product, which is used directly in the next Step.

1. extractionis then extracted with DCM
2. washThe organic phase is washed with water and with saturated aqueous NaCl solution
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customevaporated to dryness
6. customThe residue obtained
7. customis purified by flash chromatography on silica gel (SiO2; gradient DCM/AcOEt)