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Dimethylformamide → HCID 15906598、化合物

HRID 1250484
ノート
印刷プレビュー

反応式

HRID 1250484 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1.[H-].[Na+].[CH3:14][N:15]([CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:16]1[CH:21]=[C:20](Br)[N:19]=[C:18](Br)[CH:17]=1.[CH3:31][N:32]([CH:34]=[O:35])C>CCCCCC>[C:31]1([NH:32][C:34]([C:20]2[CH:21]=[C:16]([N:15]([CH3:14])[CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH:17]=[C:18]([O:9][C:5]3[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:10])([F:11])[F:1])[CH:4]=3)[N:19]=2)=[O:35])[CH:5]=[CH:4][CH:3]=[CH:8][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 73763-(Trifluoromethyl)phenolHCID 24758Sodium hydrideHCID 183262194-{Methyl(phenylmethyl)amino}-2,6-dibromo pyridine

生成物 1

HCID 15906598HCID 15906598、化合物

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

1.56 g (0.0080×1.2 mol) of 3-(trifluoromethyl) phenol was dissolved in about 20 ml of DMF. The solution was further mixed with 0.34 g (ca. 60% in mineral oil; 0.0080×1.06 mol) of NaH and then with 2.85 g (0.0080 mol) of 4-{methyl(phenylmethyl)amino}-2,6-dibromo pyridine. After treating the solution under reflux for about 6 hours, the obtained reaction solution was allowed to stand for cooling to room temperature. After the reaction solution was distributed in hexane-saturated sodium bicarbonate water, the organic phase of the obtained solution was washed with saturated brine and dried with anhydrous sodium sulfate. The resultant solution was concentrated and then purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), and the obtained eluate was subjected to recrystallization using hexane, thereby obtaining an aimed product.

後処理

  1. additionAfter treating the solution
  2. temperatureunder reflux for about 6 hours
  3. customthe obtained reaction solution
  4. washthe organic phase of the obtained solution was washed with saturated brine
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationThe resultant solution was concentrated
  7. custompurified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)
  8. customthe obtained eluate was subjected to recrystallization

出典と根拠

ORDレコード
ord-3fd6a957f7f24f0c847110546722eca7
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06339045B1

反応ノート

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