反应详情

温度

200 °C

A mixture of 0.59 g of 2-methylamino-3-propionylthiophene, 1.18 g of ethyl carbamate and 0.07 g of zinc chloride is heated at 200°C for 1 hour. After cooling, the reaction mixture is extracted with chloroform. The extracts are combined, washed with water, dried over sodium sulfate and concentrated to dryness under reduced pressure. The residue is chromatographed on silica gel using chloroform as an eluent to give 1-methyl-4-ethyl-1,2-dihydrothieno[ 2,3-d]pyrimidin-2-one as crystals having a melting point of 155.5°-156.5°C (after recrystallization from ethanol).

1. temperatureAfter cooling
2. extractionthe reaction mixture is extracted with chloroform
3. washwashed with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated to dryness under reduced pressure
6. customThe residue is chromatographed on silica gel