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Diethyl Ether → 2-[(3-Trifluoromethylphenyl)amino]-3-pyridylmethanol

HRID 2372753
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인쇄 미리보기

반응식

HRID 2372753 반응식
C(OCC)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:26])[CH:17]=1.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1.C(OCC)(=O)C>[F:30][C:28]([F:29])([F:31])[C:14]1[CH:15]=[C:16]([NH:18][C:19]2[C:20]([CH2:25][OH:26])=[CH:21][CH:22]=[CH:23][N:24]=2)[CH:17]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 135776882-[(3-Trifluoromethylphenyl)amino]-3-pyridylmethanol수율 85%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran
용매
HCID 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-c48aa1175c95456d94d2b70ee0400e9d
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05100902

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