反应详情

To a mixture of ethyl P-methyl-2-nitro-5-chlorophenylphosphinate (20.0 mmol) and thiophenol (40.0 mmol) in 20 ml of ethanol is added sodium hydroxide (60.0 mmol) in 1 ml of water. The mixture is heated under reflux for 24 hours. The reaction mixture is poured into water, acidified with dilute HCl and extracted with methylene chloride (2×). The combined extracts are washed with brine, dried and evaporated to dryness. The resulting oily residue is treated with diazomethane in methanol, concentrated and purified by preparative TLC to yield methyl P-methyl-2-nitro-5-phenylthiophenylphosphinate.

1. temperatureThe mixture is heated
2. temperatureunder reflux for 24 hours
3. extractionextracted with methylene chloride (2×)
4. washThe combined extracts are washed with brine
5. customdried
6. customevaporated to dryness
7. additionThe resulting oily residue is treated with diazomethane in methanol
8. concentrationconcentrated
9. custompurified by preparative TLC