反应详情

温度

0 °C

Ethyl N-trifluoroacetyl-N-(dichlorophosphonomethyl)glycinate (6.6 g, 0.02 mole) was dissolved in 100 ml. of ether, cooled to 0° C. and treated with a solution of methanol (0.8 g, 0.02 mole) and triethylamine (2.78 g, 0.02 mole) in 50 ml. of ether. After two hours, the solution was filtered and the filtrate cooled to 0° C. and treated with a solution of thiophenol (2.05 ml, 0.02 mole) and triethylamine (2.78 ml, 0.02 mole) in 50 ml. of ether. After two hours, the solution was filtered and the filtrate was concentrated in vacuo. The residue was extracted into petroleum ether and the petroleum ether was removed by distillation in vacuo. The residue (1.5 g) was chromatographed on silica gel eluting with ether/benzene (7/3) to afford ethyl N-trifluoroacetyl-N-(methoxy(phenylthio)phosphonomethyl)glycinate as a colorless oil (1 g), ND =1.5047.

1. filtrationthe solution was filtered
2. waitAfter two hours
3. filtrationthe solution was filtered
4. concentrationthe filtrate was concentrated in vacuo
5. extractionThe residue was extracted into petroleum ether
6. customthe petroleum ether was removed by distillation in vacuo
7. customThe residue (1.5 g) was chromatographed on silica gel eluting with ether/benzene (7/3)