反应详情

A solution of methyl 5-[(2R)-2-({(2R)-2-{[tert-butyl(dimethyl)silyl]oxy}-2-[4-hydroxy-3-(hydroxymethyl)phenyl]ethyl}amino)propyl]-1H-indole-2-carboxylate (Preparation 12, 0.30 g, 0.59 mmol) in 1,4-dioxane (10 ml) was treated with a solution of sodium hydroxide (59 mg, 1.46 mmol) in water (1 ml) and the resulting mixture left to stir at room temperature for 30 minutes. After this time the reaction mixture was heated to 90° C. for 30 minutes and then cooled to room temperature. The solvent was removed in vacuo and the residue re-dissolved in water (20 ml) and pH adjusted to 7 by addition of 2N Hydrochloric acid. The solid that formed was filtered off, solubilised in a mixture of dichloromethane and methanol (20 ml 90:10 by volume), dried (magnesium sulphate) and the solvent removed in vacuo to give the title compound as a pale orange foam.

1. waitthe resulting mixture left
2. temperatureAfter this time the reaction mixture was heated to 90° C. for 30 minutes
3. temperaturecooled to room temperature
4. customThe solvent was removed in vacuo
5. dissolutionthe residue re-dissolved in water (20 ml)
6. additionpH adjusted to 7 by addition of 2N Hydrochloric acid
7. customThe solid that formed
8. filtrationwas filtered off
9. additionsolubilised in a mixture of dichloromethane and methanol (20 ml 90:10 by volume)
10. dry with materialdried (magnesium sulphate)
11. customthe solvent removed in vacuo