Lithium Hydroxide → HCID 86658522, Verbindung

HRID 471372Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 471372
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:27]([F:30])([F:29])[F:28])[O:13][N:12]=[C:11]([C:14]3[CH:25]=[CH:24][C:17]([C:18]([N:21]([CH3:23])[CH3:22])=[N:19][OH:20])=[C:16]([CH3:26])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.[Li+].[OH-].S(OC)(O[CH3:37])(=O)=O>CN(C=O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:27]([F:28])([F:30])[F:29])[O:13][N:12]=[C:11]([C:14]3[CH:25]=[CH:24][C:17]([C:18]([N:21]([CH3:22])[CH3:23])=[N:19][O:20][CH3:37])=[C:16]([CH3:26])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1

Komponenten

6

Edukt 3

HCID 3939Lithium HydroxideHCID 6497Dimethyl SulfateHCID 1363411624-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-N'-hydroxy-2,N,N-trimethyl-benzamidine

Produkt 1

HCID 86658522HCID 86658522, VerbindungAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 4-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-N′-hydroxy-2,N,N-trimethyl-benzamidine (200 mg) in DMF (5 mL) was added a solution of LiOH (31 mg) in water (2 mL), before adding dimethyl sulfate (0.21 mL, 0.27 g). The mixture was stirred at room temperature over night and poured onto water. The aqueous layer was extracted with MTBE and the combined organic layers were washed with water, dried (Na2SO4) and evaporated to yield the title compound (170 mg, 83%).

Aufarbeitung

  1. additionpoured onto water
  2. extractionThe aqueous layer was extracted with MTBE
  3. washthe combined organic layers were washed with water
  4. dry with materialdried (Na2SO4)
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-17d0c5b2df5a4afd82bcfb079c7a05ae
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08633134B2

Notizen zur Reaktion

Wird geladen…