反应详情

Metachloroperbenzoic acid (2.79 g) is added in portions to a solution of 5-chloro-2-methyl-3-(piperidin-4-ylthio) -1H-indole (3 g, prepared in Example 15) in dichloromethane (25 ml) at -40° C. After 4 hours at room temperature, the insoluble material is filtered off. The filtrate is washed with sodium hydroxide and then with water. The aqueous phases are extracted with ether and then with ethyl acetate. The organic phases are combined, dried over magnesium sulfate and concentrated. The oily residue obtained is chromatographed on silica gel (eluent: CH2Cl2 /MeOH/NH4OH : 90/10/1) to give 5-chloro-2-methyl-3-(piperidin-4-yl-sulfinyl)-1H-indole in the form of an oil, which crystallizes on the addition of ether (0.4 g).

1. filtrationthe insoluble material is filtered off
2. washThe filtrate is washed with sodium hydroxide
3. extractionThe aqueous phases are extracted with ether
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customThe oily residue obtained
7. customis chromatographed on silica gel (eluent: CH2Cl2 /MeOH/NH4OH : 90/10/1)