反应详情

6.06 g (15 mmol) of Lawesson reagent is added to a solution of 4.15 g (25 mmol) of 4-nitrobenzamide in 100 ml of 1,4-dioxan. The reaction mixture is heated under reflux for two hours. After the solution has returned to ambient temperature, it is poured into 150 ml of water and extracted with 5 times 100 ml of ethyl acetate. The organic solution is dried over magnesium sulphate, filtered and concentrated under vacuum in order to produce a yellow oil which is purified on a silica gel column (eluant: heptane/ethyl acetate 1/1). The pure fractions are collected and concentrated under vacuum. 3.26 g of a yellow powder is obtained with a yield of 72%. Melting point: 165-167° C.

1. temperatureThe reaction mixture is heated
2. temperatureunder reflux for two hours
3. customhas returned to ambient temperature
4. extractionextracted with 5 times 100 ml of ethyl acetate
5. dry with materialThe organic solution is dried over magnesium sulphate
6. filtrationfiltered
7. concentrationconcentrated under vacuum in order
8. customto produce a yellow oil which
9. customis purified on a silica gel column (eluant: heptane/ethyl acetate 1/1)
10. customThe pure fractions are collected
11. concentrationconcentrated under vacuum