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

HRID 1108030노트

반응식

HRID 1108030 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 187003874-(2-(Methylsulfinyl)phenyl)piperidine수율 96%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5949296e1be34bedbe3dd516b08dde39
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06063926

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