Hydrochloric Acid → HCID 57747227, Verbindung

HRID 1163463Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1163463
Br[CH2:2][C:3]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=1)=[O:4].Cl[C:21]1[CH:22]=[CH:23][C:24]([O:28][C:29]2[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][C:30]=2[Cl:36])=[C:25]([OH:27])[CH:26]=1.C(=O)([O-])[O-].[K+].[K+].[ClH:43]>O1CCCC1.O>[Cl:43][C:22]1[CH:21]=[CH:26][C:25]([O:27][CH2:2][C:3]([C:5]2[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=2)=[O:4])=[C:24]([O:28][C:29]2[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][C:30]=2[Cl:36])[CH:23]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 5564TriclosanHCID 11430Potassium CarbonateHCID 6161612-Bromo-1-[3,5-di(tert-butyl)-4-hydroxyphenyl]ethan-1-one

Produkt 1

HCID 57747227HCID 57747227, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 10.0 g (30.5 mmol) of 2-bromo-1-(4-hydroxy-3,5-di-tert-butylphenyl)-ethanone and the 8.8 g (30.5 mmol) of 5-chloro-2-(2,4-di-chloro-phenoxy)-phenol in 50 ml of tetrahydrofuran, 6.3 g (45.7 mmol) of potassium carbonate is added and the mixture is stirred for 4 days at room temperature. After addition of water and adjusting the pH to 5-6 by adding 32% HCl, the mixture is extracted with ethyl acetate. The combined extracts are washed with water, dried and evaporated. Crystallization of the crude product from methanol gives 15.4 g of compound 104, m.p. 111-114° C.

Aufarbeitung

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe combined extracts are washed with water
  3. customdried
  4. customevaporated
  5. customCrystallization of the crude product from methanol

Quellen und Nachweise

ORD-Eintrag
ord-a92d71a908804df78dbae6c64069ec4b
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07820865B2

Notizen zur Reaktion

Wird geladen…