反应详情

A solution of 2.1 g (7.1 mmol) of 3-tert-butyl-4-dimethylcarbamoylsulfanyl-benzoic acid methyl ester (Example W) in toluene (100 mL) was cooled to −78° C. and treated with 42 mL of DIBAL (1.0 M in CH2Cl2; 42 mmol). The reaction mixture was allowed to warm to room temperature overnight. The reaction was quenched cautiously with saturated aqueous citric acid and extracted with EtOAc (2×100 mL). The combined organic extracts were washed with brine, dried (MgSO4), and concentrated. Chromatography of the residue over silica gel, eluting with 3:2 hexane:EtOAc, gave the title compound.

1. customThe reaction was quenched cautiously with saturated aqueous citric acid
2. extractionextracted with EtOAc (2×100 mL)
3. washThe combined organic extracts were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. washChromatography of the residue over silica gel, eluting with 3:2 hexane