反应详情

A mixture of 1-chloro-3-fluoro-propan-2-one (Step 38.3) (1.14 g, 10.3 mmol) and N-acetyl-2-thiourea (1.22 g, 10.3 mmol) in EtOH (10 mL) is stirred for 1.5 h at reflux, allowed to cool and concentrated. The residue is dissolved in DCM/H2O and extracted with DCM. The organic phase is dried (Na2SO4), filtered and concentrated. The residue is purified by silica gel column chromatography (Hex/EtOAc, 1:1) to afford 0.143 g of the title compound: ESI-MS: 173.1 [M−H]−; tR=1.98 min (System 1); TLC: Rf=0.21 (Hex/EtOAc, 1:1).

1. temperatureat reflux
2. temperatureto cool
3. concentrationconcentrated
4. dissolutionThe residue is dissolved in DCM/H2O
5. extractionextracted with DCM
6. dry with materialThe organic phase is dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue is purified by silica gel column chromatography (Hex/EtOAc, 1:1)