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Hydrochloric Acid → 4-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidine Hydrochloride

HRID 748802
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HRID 748802 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2([C:24]3[CH:29]=[C:28]([F:30])[CH:27]=[CH:26][C:25]=3[F:31])[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.Cl>ClCCl.C(O)C.C(OCC)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2([C:24]3[CH:29]=[C:28]([F:30])[CH:27]=[CH:26][C:25]=3[F:31])[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)(=[O:9])=[O:10])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 59750843t-Butyl 4-[(4-chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-1-piperidinecarboxylate

생성물 1

HCID 692029464-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidine Hydrochloride수율 199.7%

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 3283
Diethyl Ether
용매
HCID 6344Dichloromethane용매

실험 절차

In dichloromethane (100 ml) was dissolved t-butyl 4-[(4-chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-1-piperidinecarboxylate (3.17 g, 6.72 mmol), followed by the dropwise addition of trifluoroacetic acid (10.0 ml) under ice cooling. After stirring at room temperature for 2 hours, the reaction mixture was concentrated under reduced pressure. To the residue thus obtained was added a 1N solution (30 ml) of hydrochloric acid in ethanol. The resulting mixture was concentrated under reduced pressure to give a white solid. The white solid thus obtained was washed with diethyl ether, whereby the title compound (2.74 g, 6.71 mmol, quant.) was obtained as a white powder.

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customTo the residue thus obtained
  3. concentrationThe resulting mixture was concentrated under reduced pressure
  4. customto give a white solid
  5. customThe white solid thus obtained

출처 및 근거

ORD 기록
ord-d40ce85f2d2c41f698be1067ca2ff39d
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07399775B2

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