Trifluoroacetic acid → 1,2,3,6-Tetrahydro-4-(3-(methylthio)phenyl)pyridine

HRID 1483910

반응식

HRID 1483910 반응식
C(OC([N:8]1[CH2:13][CH2:12][C:11](O)([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([S:20][CH3:21])[CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:21][S:20][C:16]1[CH:15]=[C:14]([C:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH:10]=2)[CH:19]=[CH:18][CH:17]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 129889644-Hydroxy-4-(3-methylsulfanylphenyl)-piperidin-1-carboxylic acid tert-butyl ester

생성물 1

HCID 129889651,2,3,6-Tetrahydro-4-(3-(methylthio)phenyl)pyridine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-Hydroxy-4-(3-methylsulfanyl-phenyl)-piperidin-1-carboxylic acid tert-butyl ester (3.97 g) was dissolved in CH2Cl2 (500 ml) and trifluoroacetic acid (80 ml) was added in one portion. The mixture was refluxed for one hour and then washed with two portions of 10%-Na2CO3, dried (MgSO4), filtered and evaporated to dryness. Yield 2.07 g. MS m/z (relative intensity, 70 eV) 205 (M+, 73), 158 (44), 129 (95), 128 (80), 82 (bp).

후처리

  1. temperatureThe mixture was refluxed for one hour
  2. washwashed with two portions of 10%-Na2CO3
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-8ea3ec1ca05045deb71ab743ec5eb24c
출처 데이터셋
uspto-grants-2016_08
특허 번호
USRE046117E1

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