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Dichloromethane → tert-Butyl 4-[(4-{[5-({[(4-methoxy-2,6-dimethylphenyl)sulfonyl](methyl)amino}methyl)-1,3,4-oxadiazol-2-yl]carbonyl}piperazin-1-yl)methyl]piperidine-1-carboxylate

HRID 469090
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 469090
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([S:10]([N:13]([CH3:28])[CH2:14][C:15]2[O:16][C:17]([C:20]([N:22]3[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)=[O:21])=[N:18][N:19]=2)(=[O:12])=[O:11])=[C:5]([CH3:29])[CH:4]=1.[CH:30]([CH:32]1[CH2:37][CH2:36][N:35]([C:38]([O:40][C:41]([CH3:44])([CH3:43])[CH3:42])=[O:39])[CH2:34][CH2:33]1)=O.C(Cl)Cl.C(OC(=O)C)(=O)C>ClCCCl.CO>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([S:10]([N:13]([CH2:14][C:15]2[O:16][C:17]([C:20]([N:22]3[CH2:23][CH2:24][N:25]([CH2:30][CH:32]4[CH2:37][CH2:36][N:35]([C:38]([O:40][C:41]([CH3:42])([CH3:44])[CH3:43])=[O:39])[CH2:34][CH2:33]4)[CH2:26][CH2:27]3)=[O:21])=[N:18][N:19]=2)[CH3:28])(=[O:11])=[O:12])=[C:5]([CH3:29])[CH:4]=1
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Komponenten

7

Edukt 4

HCID 6344DichloromethaneHCID 7918Acetic AnhydrideHCID 1514430tert-Butyl 4-formylpiperidine-1-carboxylateHCID 583933044-Methoxy-N,2,6-trimethyl-N-{[5-(piperazin-1-ylcarbonyl)-1,3,4-oxadiazol-2-yl]methyl}benzenesulfonamide

Produkt 1

HCID 46175984
tert-Butyl 4-[(4-{[5-({[(4-methoxy-2,6-dimethylphenyl)sulfonyl](methyl)amino}methyl)-1,3,4-oxadiazol-2-yl]carbonyl}piperazin-1-yl)methyl]piperidine-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 111,2-DichloroethaneLösungsmittelHCID 887MethanolLösungsmittel

Versuchsvorschrift

4-Methoxy-N,2,6-trimethyl-N-{[5-(piperazin-1-ylcarbonyl)-1,3,4-oxadiazol-2-yl]methyl}benzenesulfonamide (0.2 g, 0.44 mmol) and tert-butyl 4-formylpiperidine-1-carboxylate (0.14 g, 0.66 mmol) were dissolved in DCE (4 mL) and a few 4 Å molecular sieves added. The reaction was stirred for 30 min at ambient temperature prior to addition of STAB (0.28 g, 1.3 mmol). The reaction was stirred for 18 h, diluted with MeOH (0.5 mL) and concentrated in vacuo. The residue was redissolved in DCM (5 mL) and filtered through Celite, washing with DCM. The DCM solution was treated with acetic anhydride (0.1 mL, 1.0 mmol) and stirred for 30 min at ambient temperature. The solvent was removed in vacuo and the residue redissolved in MeOH (2 mL) and the solution absorbed on to a 2 g SCX cartridge. The sorbent was washed with MeOH (10 mL) and the product eluted with 7 N NH3 in MeOH (10 mL). The solvent was removed in vacuo to afford the title compound.

Aufarbeitung

  1. additiona few 4 Å molecular sieves added
  2. additionto addition of STAB (0.28 g, 1.3 mmol)
  3. stirringThe reaction was stirred for 18 h
  4. concentrationconcentrated in vacuo
  5. dissolutionThe residue was redissolved in DCM (5 mL)
  6. filtrationfiltered through Celite
  7. washwashing with DCM
  8. stirringstirred for 30 min at ambient temperature
  9. customThe solvent was removed in vacuo
  10. dissolutionthe residue redissolved in MeOH (2 mL)
  11. customthe solution absorbed on to a 2 g SCX cartridge
  12. washThe sorbent was washed with MeOH (10 mL)
  13. washthe product eluted with 7 N NH3 in MeOH (10 mL)
  14. customThe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-64b1f93acff8485a91c06115aa95b1d9
Quelldatensatz
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08623859B2

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