反应详情

In a mixture of 60 ml of ethanol and 200 ml of xylene was dissolved 40 g of DL-β-hydroxyphenethylamine, and the resulting solution was added dropwise to a solution of 57.8 g of 1,1-bis(methylthio)-2-nitroethene in 600 ml of xyelene under reflux over a period of 1.5 hours to effect reaction. During the reaction, the low-boiling fractions were gradually removed by distillation and the reaction temperature was maintained at 130° C. to 140° C. After completion of the reaction, crystals were deposited with stirring under ice-cooling. The crystals deposited were collected by filtration, dried, and then mixed with 200 ml of a 5% (by weight) aqueous sodium hydroxide solution. After a slight amount of insolubles were removed by filtration, the filtrate was adjusted to pH 6 with a 10% (by weight) aqueous acetic acid solution, and the crystals deposited were collected by filtration and dried to obtain 34 g of 2-nitromethylene-5-phenyloxazolidine having a melting point of 139°-141° C.

1. temperatureunder reflux over a period of 1.5 hours
2. customreaction
3. customDuring the reaction
4. customthe low-boiling fractions were gradually removed by distillation
5. temperaturethe reaction temperature was maintained at 130° C. to 140° C
6. customAfter completion of the reaction, crystals
7. temperaturecooling
8. filtrationThe crystals deposited were collected by filtration
9. customdried
10. additionmixed with 200 ml of a 5% (by weight) aqueous sodium hydroxide solution
11. customAfter a slight amount of insolubles were removed by filtration
12. filtrationthe crystals deposited were collected by filtration
13. customdried