反应详情

A solution of 6-benzyloctahydro-1H-pyrrolo[3,4-b]pyridine (2.00 g) and 37% HCHO (6.0 mL) in HCO2H was heated to 90° C. and stirred for 4 h. The reaction mixture was cooled to rt and poured into ice-water. The mixture was adjusted to pH 10 with 2M NaOH aqueous solution and extracted with CH2Cl2 (70 mL×3). The combined organic phases were dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated in vacuo and the residue was chromatographed with a silica gel column (eluting agent: 20:1 (v/v) DCM/MeOH) to give the title compound as pale yellow oil (0.95 g, 45.00%), HPLC: 85.00%. The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 231.2 (M+1).

1. extractionextracted with CH2Cl2 (70 mL×3)
2. dry with materialThe combined organic phases were dried over anhydrous Na2SO4
3. filtrationfiltered
4. concentrationThe filtrate was concentrated in vacuo
5. customthe residue was chromatographed with a silica gel column (eluting agent: 20:1 (v/v) DCM/MeOH)