反应详情

温度

60 °C

To benzene (10 ml) was added N-[3-(4,5,7-trifluorobenzothiazol-2-yl)propionyl]-N-methylglycine ethyl ester (610 mg, 1.7 mmol) obtained in Example 3-ii) and phosphorus pentasulfide (378 mg, 1.7 mmol) and the mixture was heated at 60° C. for 3 hours. The organic phase was decanted and the residue was extracted with ether. All the organic phases were combined, washed with water, dried and evaporated to yield a residue, which was crystallized from hexane-isopropyl ether to give N-[3-(4,5,7-trifluorobenzothiazol-2-yl)-1-thioxopropyl]N-methylglycine ethyl ester (225 mg, 35%) as colorless crystals.

1. customThe organic phase was decanted
2. extractionthe residue was extracted with ether
3. washwashed with water
4. customdried
5. customevaporated
6. customto yield a residue, which
7. customwas crystallized from hexane-isopropyl ether