N-methyl-2-pyrrolidone → 2-Amino-3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridine

HRID 610187노트

반응식

HRID 610187 반응식
CN1CCCC1=O.[NH2:8][C:9]1[C:14]([F:15])=[C:13]([CH3:16])[C:12]([F:17])=[C:11](F)[N:10]=1.[CH3:19][O:20][C:21]1[CH:28]=[CH:27][C:24]([CH2:25][NH2:26])=[CH:23][CH:22]=1>C(Cl)(Cl)Cl>[NH2:8][C:9]1[C:14]([F:15])=[C:13]([CH3:16])[C:12]([F:17])=[C:11]([NH:26][CH2:25][C:24]2[CH:27]=[CH:28][C:21]([O:20][CH3:19])=[CH:22][CH:23]=2)[N:10]=1

참가 물질

5

반응물 3

HCID 13387N-methyl-2-pyrrolidoneHCID 754524-MethoxybenzylamineHCID 125080923,5,6-Trifluoro-4-methylpyridin-2-amine

생성물 1

HCID 221212712-Amino-3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridine수율 38.7%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
140 °C

실험 절차

To 3 ml of N-methylpyrrolidone were added 1.35 g of 2-amino-3,5,6-trifluoro-4-methylpyridine together with 3.0 g of p-methoxybenzylamine, and the mixture was stirred under nitrogen atmosphere at 140° C. for 18 hours and allowed to cool. After adding 30 ml of chloroform, the mixture was washed three times with 300 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to chromatography (silica gel, 20 g; eluent: chloroform:n-hexane, 1:1, and then, chloroform) to obtain 0.90 g of the title compound as a pale yellow crude oil.

후처리

  1. temperatureto cool
  2. washthe mixture was washed three times with 300 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-9354dd18568e427eab68de0ce01ea9a4
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998436

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