StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Triethylamine → HCID 178488310, Verbindung

HRID 1663263
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1663263
[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:12]2[CH:25]([CH2:26][C:27]([OH:29])=O)[C:24]3[C:19](=[C:20]([O:30][CH3:31])[CH:21]=[CH:22][CH:23]=3)[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]2=3)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.Cl.Cl.[N:65]1([CH2:70][CH2:71][C@H:72]2[CH2:77][CH2:76][C@H:75]([NH2:78])[CH2:74][CH2:73]2)[CH2:69][CH2:68][CH2:67][CH2:66]1>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:12]2[CH:25]([CH2:26][C:27]([NH:78][C@H:75]3[CH2:76][CH2:77][C@H:72]([CH2:71][CH2:70][N:65]4[CH2:69][CH2:68][CH2:67][CH2:66]4)[CH2:73][CH2:74]3)=[O:29])[C:24]3[C:19](=[C:20]([O:30][CH3:31])[CH:21]=[CH:22][CH:23]=3)[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]2=3)(=[O:10])=[O:11])[CH:5]=[CH:6][C:7]=1[Cl:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8471Triethylamine2×HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 67436621HCID 67436621, VerbindungHCID 178478709HCID 178478709, Verbindung

Produkt 1

HCID 178488310HCID 178488310, Verbindung
Ausbeute 60,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of [5-(3,4-dichloro-benzenesulfonyl)-10-methoxy-5,6-dihydro-phenanthridin-6-yl]-acetic acid (Example 17/d) (0.163 g, 0.34 mmol), triethylamine (0.3 mL, 2.1 mmol) and O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HBTU) (0.152 g, 0.4 mmol) in dry dimethyl formamide (10 mL) was stirred at room temperature for five minutes before trans-4-(2-pyrrolidin-1-yl-ethyl)-cyclohexylamine dihydrochloride (Reference Example 4) (0.09 g, 0.34 mmol) was added. The pH of the reaction mixture was adjusted to 8 by addition of triethylamine, the so obtained mixture was stirred at room temperature overnight, then concentrated in vacuo. The residue was treated with saturated sodium hydrogencarbonate solution (30 mL), the precipitated crystals were filtered off, washed with water and dried. The crude product was purified by column chromatography using Kieselgel 60 (0.040-0.063 mm) (Merck) as adsorbent, and chloroform:methanol:NH4OH=9:1:0.1 as eluent. The product was crystallized with diethyl ether to yield 0.135 g (60%) of the title compound. MS (EI) 657.2 (MH+).

Aufarbeitung

  1. additionwas added
  2. concentrationconcentrated in vacuo
  3. additionThe residue was treated with saturated sodium hydrogencarbonate solution (30 mL)
  4. filtrationthe precipitated crystals were filtered off
  5. washwashed with water
  6. customdried
  7. customThe crude product was purified by column chromatography
  8. customThe product was crystallized with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-e69ac7d8cb804e49ad1111639474146c
Quelldatensatz
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08034827B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion