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Trifluoroacetic acid → HCID 178489565, 화합물

HRID 54203
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HRID 54203 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH:15]2[CH2:20][CH2:19][C:18](O)([C:21]3[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][C:22]=3[CH3:28])[CH2:17][CH2:16]2)[CH2:11][CH2:10]1.FC(F)(F)C(O)=O>ClCCl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:10][CH2:11][N:12]([C@H:15]2[CH2:16][CH2:17][C@H:18]([C:21]3[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][C:22]=3[CH3:28])[CH2:19][CH2:20]2)[CH2:13][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 199585471-(2-Methoxyphenyl)-4-[1-hydroxy-1-(2,4-dimethylphenyl)cyclohex-4-yl]piperazine

생성물 1

HCID 178489565HCID 178489565, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(2-methoxyphenyl)-4-[1-hydroxy-1-(2,4-dimethylphenyl)cyclohex-4-yl]piperazine in dichloromethane (anhydrous) at room temperature was added trifluoroacetic acid (8 equivalents). The solution was stirred overnight. Excess trifluoroacetic acid was removed under vacuo and the residue poured into sodium bicarbonate solution. The neutralised aqueous layer was extracted with dichloromethane, washed with salt solution, dried (MgSO4) and filtered. The solvent was removed and the residue purified by silica gel pressure column chromatography using hexane/ether (2/1) as eluant. The solid residue was recrystallised from ether to give the title compound which was converted to its dihydrochloride, m.p. 219° C. (dec.).

후처리

  1. customExcess trifluoroacetic acid was removed under vacuo
  2. additionthe residue poured into sodium bicarbonate solution
  3. extractionThe neutralised aqueous layer was extracted with dichloromethane
  4. washwashed with salt solution
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe solvent was removed
  8. customthe residue purified by silica gel pressure column chromatography
  9. customThe solid residue was recrystallised from ether

출처 및 근거

ORD 기록
ord-20af70c701d14953a299c24e96943a4a
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05622951

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