Trifluoroacetic acid → 4-(2-(Methylsulfinyl)phenyl)piperidine

HRID 1108030ノート

反応式

HRID 1108030 の反応式
C(OC([N:11]1[CH2:16][CH2:15][CH:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[S:23]([CH3:25])=[O:24])[CH2:13][CH2:12]1)=O)C1C=CC=CC=1.FC(F)(F)C(O)=O>C1(C)C=CC=CC=1>[CH3:25][S:23]([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[CH:14]1[CH2:15][CH2:16][NH:11][CH2:12][CH2:13]1)=[O:24]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 226222471-Benzyloxycarbonyl-4-(2-methylsulfinylphenyl)piperidine

生成物 1

HCID 187003874-(2-(Methylsulfinyl)phenyl)piperidine収率 96%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

The product of Step 4 (0.5 g) was treated with trifluoroacetic acid (10 mL) and heated at reflux temperature for 45 minutes. The reaction mixture was cooled, diluted with toluene (40 mL) and evaporated. This procedure was repeated two more times. The residue was treated with CH2Cl2 (70 mL) and adjusted to alkaline pH via addition of NH4OH solution. The organic layer was separated, dried over MgSO4, filtered and evaporated to give 4-(2-methylsulfinylphenyl)piperidine (0.3 g).

後処理

  1. temperatureheated
  2. temperatureat reflux temperature for 45 minutes
  3. temperatureThe reaction mixture was cooled
  4. customevaporated
  5. additionThe residue was treated with CH2Cl2 (70 mL)
  6. additionvia addition of NH4OH solution
  7. customThe organic layer was separated
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated

出典と根拠

ORDレコード
ord-5949296e1be34bedbe3dd516b08dde39
出典データセット
uspto-grants-2000_05
特許番号
US06063926

反応ノート

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