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

HRID 654759노트

반응식

HRID 654759 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 86746009(3-Trifluoromethylphenyl)amino-3-pyridylmethanol수율 85%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-adec0c6b3a39477ebb5af8ba95e14237
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05134147

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