Triethylamine → HCID 68756210, Verbindung

HRID 872206Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 872206
C(N(CC)CC)C.[F:8][C:9]([F:14])([F:13])[C@@H:10]([OH:12])[CH3:11].Cl[C:16]([O:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1)=[O:17]>CN(C)C1C=CN=CC=1.ClCCl>[F:8][C:9]([F:14])([F:13])[C@@H:10]([O:12][C:16](=[O:17])[O:18][C:19]1[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=1)[CH3:11]

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 821294-Nitrophenyl chloroformateHCID 6999971(2S)-1,1,1-Trifluoropropan-2-ol

Produkt 1

HCID 68756210HCID 68756210, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Triethylamine (2.3 mL) is added to a solution of 4-dimethylaminopyridine (13 mg), (S)-1,1,1-trifluoro-propan-2-ol (75% in tert-butyl methyl ether; 2.00 g), and 4-nitrophenyl chloroformate (2.90 g) in dichloromethane (80 mL) chilled in an ice bath. The solution is stirred in the cooling bath for 30 min and then at room temperature overnight. The solution is washed with 10% aqueous K2CO3 solution and water and dried (MgSO4). The solvent is evaporated and the residue is chromatographed on silica gel (dichloromethane) to give the title compound.

Aufarbeitung

  1. temperaturechilled in an ice bath
  2. customat room temperature
  3. customovernight
  4. washThe solution is washed with 10% aqueous K2CO3 solution and water
  5. dry with materialdried (MgSO4)
  6. customThe solvent is evaporated
  7. customthe residue is chromatographed on silica gel (dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-caff9032d4db43b69739e4b24baae42a
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08975277B2

Notizen zur Reaktion

Wird geladen…