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N-methyl-2-pyrrolidone → 2-Amino-3,5-difluoro-6-(p-methoxybenzylamino)pyridine

HRID 368400
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인쇄 미리보기

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HRID 368400 반응식
CN1CCCC1=O.[NH2:8][C:9]1[C:14]([F:15])=[CH:13][C:12]([F:16])=[C:11](F)[N:10]=1.[CH3:18][O:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24][NH2:25])=[CH:22][CH:21]=1>C(Cl)(Cl)Cl>[NH2:8][C:9]1[C:14]([F:15])=[CH:13][C:12]([F:16])=[C:11]([NH:25][CH2:24][C:23]2[CH:26]=[CH:27][C:20]([O:19][CH3:18])=[CH:21][CH:22]=2)[N:10]=1
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참가 물질

5

반응물 3

HCID 13387N-methyl-2-pyrrolidoneHCID 754524-MethoxybenzylamineHCID 125080743,5,6-Trifluoropyridin-2-amine

생성물 1

HCID 221212562-Amino-3,5-difluoro-6-(p-methoxybenzylamino)pyridine수율 64.4%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
140 °C

실험 절차

To 10 ml of N-methylpyrrolidone were added 3.90 g of 2-amino-3,5,6-trifluoropyridine and 7.60 g of p-methoxybenzylamine, and the mixture was stirred under nitrogen atmosphere at 140° C. for one day and allowed to cool. To the solution was added 50 ml of chloroform, and the solution was washed three times with 500 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and the residue was subjected to chromatography (silica gel, 32 g; eluent: chloroform) to obtain 4.50 g of the title compound as a pale yellow crude oil.

후처리

  1. temperatureto cool
  2. washthe solution was washed three times with 500 ml of distilled water
  3. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-63d921abb72d410f952ae7750a5fbeb8
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06133284

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