反应详情

Potassium hydroxide (12.55 g, 224 mmol) was added to the vigorously stirred solution of methylthiopseudourea.H2SO4 (14.57 g, 52 mmol) in water (80 ml). Ethyl (4-methyl)benzoylacetate (20.0 g, 97 mmol) (obtained in preparation 1) was added to it and stirred at room temperature for 18 hours. The solid thus obtained was filtered, washed with water, ether and dried at 60° C. in vacuum to yield the title compound (1.85 g, 9.5%). 1H-NMR (DMSO-d6): δ 2.37 (s, 3H), 6.46 (s, 1H), 7.33-7.35 (d, 2H), 7.76-7.78 (d, 2H), 7.91 (bs, 2H, D2O exchangeable). MS m/z: 203.1 (M+).

1. customThe solid thus obtained
2. filtrationwas filtered
3. washwashed with water, ether
4. customdried at 60° C. in vacuum