反应详情

Acetic acid (133 μL) and NaBH3CN (14.8 mg, 0.235 mmol) were added to a stirred solution of 5-chloro-4-(tetrahydro-pyran-2-yloxymethyl)-pyridine-3-carbaldehyde (40 mg, 0.157 mmol) and 2,2-dimethyl-1,3-dioxolane-4-methanamine (203 μL, 1.57 mmol) in MeOH (1 mL). After stirring for 2 h at room temperature the solvent was removed in vacuo and the residue was partitioned between DCM (10 mL) and saturated NaHCO3 solution (10 mL). After extraction of the aqueous layer with DCM (2×10 mL) the combined organic layers were dried over Na2SO4, filtered, and concentrated in vacuo. The resulting title compound was used for the next reaction without purification. MS (m/z): 370.9 [M+H+].

1. customwas removed in vacuo
2. customthe residue was partitioned between DCM (10 mL) and saturated NaHCO3 solution (10 mL)
3. extractionAfter extraction of the aqueous layer with DCM (2×10 mL) the combined organic layers
4. dry with materialwere dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe resulting title compound was used for the next reaction without purification