反应详情

To 2,6-di-tert-butyl-4-(piperidin-4-ylsulfanyl)-phenol hydrochloride (Ex. 3c, 280 mg, 0.78 mmol) in 5 mL of dichloromethane was added triethylamine (240 mg, 2.37 mmol). The mixture was stirred for 3 min followed by the addition of 5-chlorosulfonyl-furan-2-carboxylic acid methyl ester (210 mg, 0.94 mmol). The stirring was continued for 2 h at room temperature and then the reaction was quenched with 20 mL of saturated NaH2PO4. The mixture was extracted with Ethyl acetate (40 mL) and the organic phase was dried over Na2SO4 and concentrated under reduced pressure. Chromatography (3-50% Ethyl acetate/hexanes) gave 5-[4-(3,5-di-tert-butyl-4-hydroxy-phenylsulfanyl)-piperidine-1-sulfonyl]-furan-2-carboxylic acid methyl ester as a clear oil (295 mg, 74%). ESI/CI-MS m/z 508 ([M−H]−).

1. waitThe stirring was continued for 2 h at room temperature
2. customthe reaction was quenched with 20 mL of saturated NaH2PO4
3. extractionThe mixture was extracted with Ethyl acetate (40 mL)
4. dry with materialthe organic phase was dried over Na2SO4
5. concentrationconcentrated under reduced pressure