N-Ethylaniline → 4,5-dichloro-6-(N-ethyl-N-phenylamino)pyrimidine

HRID 1592285

반응식

HRID 1592285 반응식
Cl[C:2]1[C:7]([Cl:8])=[C:6]([Cl:9])[N:5]=[CH:4][N:3]=1.[CH2:10]([NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH3:11]>C(O)C>[Cl:9][C:6]1[C:7]([Cl:8])=[C:2]([N:12]([CH2:10][CH3:11])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:3]=[CH:4][N:5]=1

참가 물질

4

반응물 2

HCID 7670N-EthylanilineHCID 2490074,5,6-Trichloropyrimidine

생성물 1

HCID 225996934,5-dichloro-6-(N-ethyl-N-phenylamino)pyrimidine수율 114%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 2 ml of ethanol were added 0.3 g of 4,5,6-trichloropyrimidine and 0.5 g of N-ethylaniline, followed by heating under reflux for 8 hours. The reaction mixture was then left for cooling to room temperature and concentrated under reduced pressure. The residue was added water and extracted three times with t-butyl methyl ether. The organic layers were combined, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.5 g of 4,5-dichloro-6-(N-ethyl-N-phenylamino)pyrimidine.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 8 hours
  3. waitThe reaction mixture was then left
  4. concentrationconcentrated under reduced pressure
  5. additionThe residue was added water
  6. extractionextracted three times with t-butyl methyl ether
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2a8cf03c371f47ca912f60d1a5896b74
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07291730B2

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