反应详情

Dissolve 3-{4-[2-(4-chloro-phenyl)-4-oxo-6,7-dihydro-4H-thiazolo[5,4-c]pyridin-5-yl]-2-methoxy-phenoxy}-azetidine-1-carboxylic acid tert-butyl ester (3.33 g, 6.16 mmol) in CH2Cl2 (21 mL) and add trifluoroacetic acid (7.25 mL). Stir for one hour at room temperature and then add 1 N NaOH to adjust to pH=8-10. Extract with EtOAc (3×50 mL) and wash with water (2×50 mL). Collect an off-white solid via vacuum filtration (2.15 g, 79%). Re-dissolve a portion of the crude material (300 mg, 0.68 mmol) in CHCl3 and add 4 N HCl/dioxane solution (about 200 μL). Remove the organic solvent via reduced pressure to dryness to give 316 mg of the titled compound. ES/MS m/z (35Cl) 442.0 [M+1]+.

1. extractionExtract with EtOAc (3×50 mL)
2. washwash with water (2×50 mL)
3. customCollect an off-white solid
4. filtrationvia vacuum filtration (2.15 g, 79%)
5. customRemove the organic solvent via reduced pressure to dryness