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4-Chlorobenzenesulfonyl chloride → (3R)-1-[(4-chlorophenyl)sulfonyl]-3-methylpiperazine

HRID 41302
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HRID 41302 반응식
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][CH2:4][N:3]1C(OC(C)(C)C)=O.C(N(CC)CC)C.[Cl:22][C:23]1[CH:28]=[CH:27][C:26]([S:29](Cl)(=[O:31])=[O:30])=[CH:25][CH:24]=1>C(Cl)Cl>[Cl:22][C:23]1[CH:28]=[CH:27][C:26]([S:29]([N:6]2[CH2:5][CH2:4][NH:3][C@H:2]([CH3:1])[CH2:7]2)(=[O:31])=[O:30])=[CH:25][CH:24]=1
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참가 물질

5

반응물 3

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 8471TriethylamineHCID 10262201tert-Butyl (2R)-2-methylpiperazine-1-carboxylate

생성물 1

HCID 11630465(3R)-1-[(4-chlorophenyl)sulfonyl]-3-methylpiperazine수율 78.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1,1-dimethylethyl (2R)-2-methyl-1-piperazinecarboxylate (1.5 g, 07.5 mmol) in dry DCM (40 mL) was added triethylamine (2.59 mL, 18.8 mmol) and 4-chlorobenzenesulfonyl chloride (3.15 g, 10.5 mmol) and the reaction stirred at room temperature for 48 h. To the reaction was added resin supported-triamine (5 g) and the mixture stirred for 4 h. The reaction mixture was filtered and the filtrate washed with 0.5 M HCl (aq., 100 mL) followed by water (100 mL) before it was dried (MgSO4), filtered and the solvent removed in vacuo. The crude product was dissolved in DCM (40 mL) and TFA (10 mL) was added. The solution was stirred for 20 min. The solvent was evaporated and the residue tajen up in DCM (40 mL) and washed with 50% aqueous sodium bicarbonate (100 mL) followed by water (100 mL). The organic phase was dried (MgSO4), filtered and the solvent removed in vacuo to give the title compound (1.62 g).

후처리

  1. additionTo the reaction was added resin
  2. stirringthe mixture stirred for 4 h
  3. filtrationThe reaction mixture was filtered
  4. washthe filtrate washed with 0.5 M HCl (aq., 100 mL)
  5. dry with materialwas dried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent removed in vacuo
  8. dissolutionThe crude product was dissolved in DCM (40 mL)
  9. additionTFA (10 mL) was added
  10. stirringThe solution was stirred for 20 min
  11. customThe solvent was evaporated
  12. washthe residue tajen up in DCM (40 mL) and washed with 50% aqueous sodium bicarbonate (100 mL)
  13. dry with materialThe organic phase was dried (MgSO4)
  14. filtrationfiltered
  15. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-d72421402bcd411a95caa05e81703400
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08530478B2

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