反应详情

温度

60 °C

To a solution of Methyl 2-[2-methyl-4-(5-chlorochroman-6-yl)-5,6,7,8-tetrahydro[1]benzothieno[2,3-b]pyridin-3-yl]-2-tert-butoxyacetate (0.027 g; 0.053 mmol) in methanol (0.9 mL) was added a solution of sodium hydroxide 10 N (0.090 mL; 0.90 mmol) and the mixture was heated to 60° C. for 18 h. The volatiles were removed under reduced pressure and the residue was dissolved in water, the mixture was then acidified by adding 1N HCl until a precipitate was formed. The solid was filtered, washed with water and dried under reduced pressure. Purification by preparative HPLC (HPLC method 1) furnished 0.005 g (18%) of the title compound as a white solid.

1. customThe volatiles were removed under reduced pressure
2. dissolutionthe residue was dissolved in water
3. additionby adding 1N HCl until a precipitate
4. customwas formed
5. filtrationThe solid was filtered
6. washwashed with water
7. customdried under reduced pressure
8. customPurification by preparative HPLC (HPLC method 1)