反应详情

To a solution of quinoline-6-carboxylic acid (1.00 g, 5.77 mmol) in MeOH (10 mL) was added hydrogen chloride (2.00 mL, 8.00 mmol) (4.0M in 1,4-dioxane). The reaction was stirred 18 h at rt, LCMS shows <10% conversion. Additional hydrogen chloride (2.00 mL, 8.00 mmol) was added and the reaction heated to 50° C. in an oil bath 36 h. The reaction was cooled to rt and concentrated in vacuo. The solid was dissolved in DCM and extracted with sat. aqueous NaHCO3 (2×50 mL). The organic layer was dried (MgSO4), and concentrated to give the product which was used without further purification in the next step.

1. temperaturethe reaction heated to 50° C. in an oil bath 36 h
2. temperatureThe reaction was cooled to rt
3. concentrationconcentrated in vacuo
4. dissolutionThe solid was dissolved in DCM
5. extractionextracted with sat. aqueous NaHCO3 (2×50 mL)
6. dry with materialThe organic layer was dried (MgSO4)
7. concentrationconcentrated
8. customto give the product which
9. customwas used without further purification in the next step