Ammonia → Bis(2-pyridyl)methylamine

HRID 1079275

반응식

HRID 1079275 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=[N:14]O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=1.N>[Zn].C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]([NH2:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=1

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 73805Di-2-pyridinylmethanone oxime

생성물 1

HCID 11106041Bis(2-pyridyl)methylamine수율 86%

시약·촉매·용매 2

HCID 23994Zinc촉매2회HCID 702Ethanol용매

실험 절차

To pyridyl ketone oxime (3 g, 15.1 mmol) was added ethanol (15 ml), concentrated ammonia solution (15 mL) and NH4OAc (1.21 g, 15.8 mmol). The solution was warmed until reflux. To this solution was added 4.64 g Zn in small portions. After the addition of all Zn, the mixture was refluxed for 1 h. and allowed to cool to ambient temperature. The solution was filtered and water (15 ml) was added. Solid NaOH was added until PH>>10 and the solution was extracted with CH2Cl2 (3×20 ml). The organic layers were dried over Na2SO4 and evaporated until dryness. Bis(pyridin-2-yl)methylamine (2.39 g, 12.9 mmol) was obtained as a colourless oil in 86% yield, showing the following analytical characteristics:

후처리

  1. temperatureThe solution was warmed
  2. temperatureuntil reflux
  3. temperaturethe mixture was refluxed for 1 h.
  4. filtrationThe solution was filtered
  5. additionwater (15 ml) was added
  6. additionSolid NaOH was added until PH>>10
  7. extractionthe solution was extracted with CH2Cl2 (3×20 ml)
  8. dry with materialThe organic layers were dried over Na2SO4
  9. customevaporated until dryness

출처 및 근거

ORD 기록
ord-02d2bd2eca3d4700aa1cbc4f2e0f85ad
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580485

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