Carbon tetrabromide → HCID 68514522, Verbindung

HRID 1717391Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1717391
O[CH2:2][CH2:3][CH2:4][C:5]1[N:9]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([NH:18][CH2:19][C:20]([F:23])([F:22])[F:21])=[O:17])=[CH:12][CH:11]=2)[N:8]=[N:7][C:6]=1[C:24]([NH2:26])=[O:25].C1(P([C:40]2[CH:45]=[CH:44]C=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Br:46]C(Br)(Br)Br>ClCCl>[Br:46][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([C:10]2[CH:11]=[CH:12][C:13]([C:16]([NH:18][CH2:19][C:20]([F:22])([F:21])[F:23])=[O:17])=[CH:14][CH:15]=2)[N:8]=[N:7][C:6]=1[C:24]([NH:26][CH:44]1[CH2:45][CH2:40]1)=[O:25]

Komponenten

5

Edukt 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 57665111HCID 57665111, Verbindung

Produkt 1

HCID 68514522HCID 68514522, VerbindungAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 5-(3-hydroxypropyl)-1-(4-{[(2,2,2-trifluoroethyl)amino]carbonyl}phenyl)-1H-1,2,3-triazole-4-carboxamide (381 mg, 0.93 mmol) obtained in Example 398 and triphenylphosphine (365 mg) in dichloromethane (12 ml) was added tetrabromomethane (460 mg), and the mixture was stirred at room temperature for 15 hr. The reaction mixture was concentrated under reduced pressure, and the obtained residue was purified by silica gel column (hexane/ethyl acetate=20/1 to 2/5) to give the title compound as a colorless solid (219 mg, 50%).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe obtained residue was purified by silica gel column (hexane/ethyl acetate=20/1 to 2/5)

Quellen und Nachweise

ORD-Eintrag
ord-6bc6c0c2213d4403a1df2e92fc6bd5f3
Quelldatensatz
uspto-grants-2010_09
Patentnummer
US07803822B2

Notizen zur Reaktion

Wird geladen…