Diethyl Ether → (3-Trifluoromethylphenyl)amino-3-pyridylmethanol

HRID 654759ノート

反応式

HRID 654759 の反応式
C([O:3]CC)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:12]1[CH:13]=[C:14]([C:28]([F:31])([F:30])[F:29])[CH:15]=[C:16]([NH:18][C:19]2[N:24]=[CH:23][CH:22]=[CH:21][C:20]=2[C:25](O)=O)[CH:17]=1.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1.C(OCC)(=O)C>[F:29][C:28]([F:31])([F:30])[C:14]1[CH:15]=[C:16]([NH:18][CH:19]([C:20]2[CH:25]=[N:24][CH:23]=[CH:22][CH:21]=2)[OH:3])[CH:17]=[CH:12][CH:13]=1

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 4488Niflumic AcidHCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 86746009(3-Trifluoromethylphenyl)amino-3-pyridylmethanol収率 85%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

500 ml of anhydrous ethyl ether are run gently onto 26 g of lithium aluminum hydride, and 100 g of niflumic acid, dissolved in 250 ml of anhydrous tetrahydrofuran, are then added dropwise. The mixture is then brought to reflux for 3 hours. After cooling, it is hydrolyzed with 150 ml of ethyl acetate and 100 ml of saturated sodium sulfate solution. After filtration, the filtrate is concentrated to obtain the expected compound in the form of a yellow solid.

後処理

  1. additionare then added dropwise
  2. temperatureto reflux for 3 hours
  3. temperatureAfter cooling
  4. filtrationAfter filtration
  5. concentrationthe filtrate is concentrated

出典と根拠

ORDレコード
ord-adec0c6b3a39477ebb5af8ba95e14237
出典データセット
uspto-grants-1992_07
特許番号
US05134147

反応ノート

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