Cyanuric chloride → 4,6-Dichloro-N,N-dihexyl-1,3,5-triazin-2-amine

HRID 1070441

반응식

HRID 1070441 반응식
[CH2:1]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[N:14]1[C:21]([Cl:22])=[N:20][C:18](Cl)=[N:17][C:15]=1[Cl:16].C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C.C(OCC)(=O)C.O>[Cl:16][C:15]1[N:14]=[C:21]([Cl:22])[N:20]=[C:18]([N:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[N:17]=1

참가 물질

7

반응물 3

HCID 7954Cyanuric chlorideHCID 8920DihexylamineHCID 10340Sodium Carbonate

생성물 1

HCID 105206134,6-Dichloro-N,N-dihexyl-1,3,5-triazin-2-amine

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

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 get (elution with 3:1 hexanes:chloroform) to afford 2,4-dichloro-6-dihexylamino-1,3,5-triazine.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 16 h
  3. customto col to ambient temperature
  4. customThe phases were separated
  5. washthe organic phase was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe crude material was purified by flash column chromatography through silica
  9. customget
  10. wash(elution with 3:1 hexanes:chloroform)

출처 및 근거

ORD 기록
ord-a4686081c0ed40b28d39d2922f8d2af7
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903088B2

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