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

HRID 1483910

反応式

HRID 1483910 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8ea3ec1ca05045deb71ab743ec5eb24c
出典データセット
uspto-grants-2016_08
特許番号
USRE046117E1

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