反应详情

A mixture of 4-(chloromethyl)-1-methyl-1H-pyrazole (2.0 g, 15 mmol) (prepared according to Intermediate 5 Step A) and sodium ethanethiolate (2.6 g, 31 mmol) in N,N-dimethylformamide (20.0 mL) was stirred at room temperature overnight. The reaction mixture was quenched with brine and extracted with EtOAc (3×). The combined extracts were dried over Na2SO4, filtered and concentrated under reduced pressure to give an oil residue which was purified by combi-flash chromatography eluted with 20% EtOAc in hexane to give 1.9 g (79% yield) of the desired product. LC-MS found: 157.1 (M+H)+.

1. customThe reaction mixture was quenched with brine
2. extractionextracted with EtOAc (3×)
3. dry with materialThe combined extracts were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customto give an oil residue which
7. customwas purified by combi-flash chromatography
8. washeluted with 20% EtOAc in hexane