Acetic Acid → HCID 66921947, Verbindung

HRID 1361470Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1361470
II.C(O)(=O)C.P(=O)(O)(O)O.[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]([C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=2)=O)=[C:15]([Cl:28])[CH:14]=1>C(OCC)(=O)C.O>[Cl:28][C:15]1[CH:14]=[C:13]([CH:18]=[CH:17][C:16]=1[CH2:19][C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=1)[NH2:12]

Komponenten

7

Edukt 4

HCID 176Acetic Acid2×HCID 807IodineHCID 1004Phosphoric AcidHCID 30165104-Amino-2,4'-dichlorobenzophenone

Produkt 1

HCID 66921947HCID 66921947, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Iodine (1 g) and 50 mL of acetic acid were mixed together, 2.53 g of 50% phosphoric acid was added thereto, and the mixture was heated with stirring to reflux. Subsequently, a mixture composed of 3.2 g of (4-amino-2-chlorophenyl)-(4′-chlorophenyl)methanone and 15 mL of acetic acid were added dropwise to the mixed solution. This solution was heated under reflux for 134 hr, was then cooled and was poured into water. Ethyl acetate was added to the mixed solution followed by separation and washing with brine. The ethyl acetate layer was concentrated to give 3.0 g of 3-chloro-4-(4-chlorobenzyl)aniline (yield 100%).

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureto reflux
  3. additionwere added dropwise to the mixed solution
  4. temperatureThis solution was heated
  5. temperatureunder reflux for 134 hr
  6. temperaturewas then cooled
  7. customfollowed by separation
  8. washwashing with brine
  9. concentrationThe ethyl acetate layer was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-7ce953cc1aa84ee8b28dbd47419eca39
Quelldatensatz
uspto-grants-2011_02
Patentnummer
US07880006B2

Notizen zur Reaktion

Wird geladen…