反应详情

16 ml of a 36% aqueous formaldehyde solution was added dropwise to a stirred solution of 4.1 g of 2D in 75 ml of dimethylformamide. The temperature of the mixture rose from 22° C. to 27° C. The mixture was stirred for 30 minutes, then 8 ml of a 40% solution of methylamine in water was added, drop-by-drop. The temperature of the mixture rose from 27° C. to 36° C. The mixture was refluxed for 3 hours, then the solvent was evaporated under reduced pressure. The residue was mixed with cold water, and the resulting mixture was extracted with ether. The solvent was evaporated from the extract, and the residue was crystallized when hexane was added, to give 2, as a white solid, m.p.: 49°-50° C.

1. customrose from 22° C. to 27° C
2. customrose from 27° C. to 36° C
3. temperatureThe mixture was refluxed for 3 hours
4. customthe solvent was evaporated under reduced pressure
5. additionThe residue was mixed with cold water
6. extractionthe resulting mixture was extracted with ether
7. customThe solvent was evaporated from the extract
8. customthe residue was crystallized when hexane
9. additionwas added
10. customto give 2