反应详情

A solution of 2.1 g (11 mmol) of 4-isopropyl-thiazole-2-carboxylic acid ethyl ester (J. Med. Chem., 1998:602-617) in CH2Cl2 (50 mL) was cooled to −78° C. under nitrogen and treated dropwise with DIBAL (12 mL of 1.0 M in CH2Cl2; 12 mmol). The mixture was stirred at low temperature for 1 hour and then treated with another 7 mL of DIBAL. The solution was stirred for 30 minutes at −78° C. H2O was added, and the mixture was extracted with EtOAc (3×100 mL). The combined extracts were washed with brine, dried (MgSO4), and concentrated. Chromatography of the residue over silica gel, eluting with 3:1 hexane:EtOAc, gave the title compound.

1. stirringThe solution was stirred for 30 minutes at −78° C
2. extractionthe mixture was extracted with EtOAc (3×100 mL)
3. washThe combined extracts were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. washChromatography of the residue over silica gel, eluting with 3:1 hexane