反应详情

A mixture of benzoylacetonitrile (1.45 g, 10 mmole), 2,5-dihydroxy-1,4-dithiane (0.76 g, 5 mmole) and diethylamine (0.73 g=1.04 mL, 10 mmole) in 4 mL absolute ethanol was heated in a teflon-sealed pressure tube for 4 hours at 50° C. with frequent stirring on a vortex mixer. By 2 hours starting materials had dissolved and shortly thereafter product began to crystallize. After refrigerating the tube overnight, the product was filtered off and washed with a little methanol to give bright yellow crystals. Yield 1.3 g, 64% 1H NMR (CDCl3) δ: 6.14 (d, 1H, H-5), 6.88 (d, 1H, H-4), 6.95 (br s, 2H, NH2), 7.5-7.7 (m, 5H, C6H5).

1. customsealed pressure tube for 4 hours at 50° C.
2. dissolutionmaterials had dissolved
3. customto crystallize
4. customthe tube overnight
5. filtrationthe product was filtered off
6. washwashed with a little methanol
7. customto give bright yellow crystals