反应详情

温度

65 °C

Under a nitrogen atmosphere 2-hydroxypropanimidamide hydrochloride (4.97 g) was suspended in dry N,N-dimethylformamide (25 mL) and sodium hydride (1.66 g, 60 wt % in mineral oil) was added in one portion. When gas evolution ceased the white suspension was heated to 65° C. After 1 h dimethyl cyanocarbonimidodithioate (6.24 g) was added and the mixture was stirred at 65° C. for 18 hours. The reaction mixture was concentrated and triturated with water (200 mL). The resulting precipitate was filtered off, washed with water and the aqueous layer was extracted with 5% methanol in dichloromethane (3×100 mL). The combined organic extracts were dried (sodium sulfate) and concentrated before being purified by flash chromatography eluting with 10% methanol in dichloromethane to give the title compound (300 mg) as a yellow oil that solidified on standing.

1. concentrationThe reaction mixture was concentrated
2. customtriturated with water (200 mL)
3. filtrationThe resulting precipitate was filtered off
4. washwashed with water
5. extractionthe aqueous layer was extracted with 5% methanol in dichloromethane (3×100 mL)
6. dry with materialThe combined organic extracts were dried (sodium sulfate)
7. concentrationconcentrated
8. custombefore being purified by flash chromatography
9. washeluting with 10% methanol in dichloromethane