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

HRID 610171
ノート
印刷プレビュー

反応式

HRID 610171 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
140 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b9e99b17a63740b2bf5101505826d631
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998436

反応ノート

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