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1-Hydroxybenzotriazole → HCID 68818466, Verbindung

HRID 734328
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 734328
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:17]([O:24][C:25]([N:27]1[CH2:32][CH2:31][NH:30][C@@H:29]([CH3:33])[CH2:28]1)=[O:26])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C1C=CC2N(O)N=NC=2C=1.CCN(CC1C=CC=CC=1)CC.C=CC1C=CC=CC=1.C=CC1C=CC(C=C)=CC=1>C(Cl)Cl.C(Cl)CCl>[CH2:17]([O:24][C:25]([N:27]1[CH2:32][CH2:31][N:30]([C:14]([CH:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:13][CH2:12]2)=[O:16])[C@@H:29]([CH3:33])[CH2:28]1)=[O:26])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 757711-HydroxybenzotriazoleHCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acidHCID 7578289(S)-Benzyl 3-methylpiperazine-1-carboxylateHCID 16212021N-benzyl-N-ethylethanamine;1,4-bis(ethenyl)benzene;styrene

Produkt 1

HCID 68818466HCID 68818466, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 111,2-DichloroethaneLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

1-(tert-Butoxycarbonyl)-piperidine4-carboxylic acid (0.53 g), (S)-1-benzyloxycarbonyl-3-methylpiperazine (D19)(0.5 g), HOBt (0.29 g) and diethylaminomethyl polystyrene (1.78 g) were stirred in DCM (30 ml), then EDC (0.53 g) was added and the reaction was stirred at rt ovemight. The mixture was filtered and washed with saturated sodium hydrogen carbonate solution (3×50 ml) and brine (30 ml). The organic layer was dried (MgSO4) and evaporated to give a crude yellow oil which was purified by chromatography [silica gel; 0-100% ethyl acetate/hexane) to give the tide compound (D20) as a clear oil which crystallised on standing (0.88 g).

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. washwashed with saturated sodium hydrogen carbonate solution (3×50 ml) and brine (30 ml)
  3. dry with materialThe organic layer was dried (MgSO4)
  4. customevaporated
  5. customto give a crude yellow oil which
  6. customwas purified by chromatography [silica gel
  7. custom0-100% ethyl acetate/hexane) to give the tide compound (D20) as a clear oil which
  8. customcrystallised

Quellen und Nachweise

ORD-Eintrag
ord-a9d13b3a961346c3b33f3099d5c8fce9
Quelldatensatz
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07592347B2

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