반응 #582219
ord-115d232797444d9f890f7b0db0772b62
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The reaction mixture was heated
- 2온도to reflux for 16 h
- 3기타to col to ambient temperature
- 4기타The phases were separated
- 5세척the organic phase was washed with brine
- 6건조dried over magnesium sulfate
- 7농축concentrated under reduced pressure
- 8기타The crude material was purified by flash column chromatography through silica gel (elution with 3:1 hexanes:chloroform)
실험 절차
Dihexylamine (6.3 mL, 27 mmol) was added to a mixture of cyanuric chloride (5.0 g, 27 mmol) and sodium carbonate (2.9 g, 27 mmol) in acetonitrile (50 mL). The reaction mixture was heated to reflux for 16 h and then allowed to col to ambient temperature. The mixture was diluted with ethyl acetate and water. The phases were separated and the organic phase was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The crude material was purified by flash column chromatography through silica gel (elution with 3:1 hexanes:chloroform) to afford 2,4-dichloro-6-dihexylamino-1,3,5-triazine.