(e)-n-[4-(3-Bromo-propyl)-3-chloro-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide → (e)-n-[3-Chloro-4-(3-diethylamino-propyl)-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide

HRID 898631Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 898631
Br[CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:26])/[CH:13]=[CH:14]/[C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][C:16]=2[Cl:25])=[CH:7][C:6]=1[Cl:27]>C(NCC)C.CCOC(C)=O>[Cl:27][C:6]1[CH:7]=[C:8]([NH:11][C:12](=[O:26])/[CH:13]=[CH:14]/[C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][C:16]=2[Cl:25])[CH:9]=[CH:10][C:5]=1[CH2:4][CH2:3][CH2:2][N:11]([CH2:12][CH3:13])[CH2:8][CH3:7]

Komponenten

4

Edukt 1

HCID 87610233(e)-n-[4-(3-Bromo-propyl)-3-chloro-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide

Produkt 1

HCID 59691692(e)-n-[3-Chloro-4-(3-diethylamino-propyl)-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8021DiethylamineLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of 0.290 g (0.603 mmol) (E)-N-[4-(3-bromo-propyl)-3-chloro-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide (Z45d) in 2 mL diethylamine was heated to 100° C. in a sealed reaction vessel in the microwave for 5 min. The reaction mixture was diluted with EtOAc, the org. phase was washed with water, dried over sodium sulphate and evaporated down i. vac. The residue was triturated with ether, the precipitate was filtered off, washed with ether and dried in a HV.

Aufarbeitung

  1. washphase was washed with water
  2. dry with materialdried over sodium sulphate
  3. customevaporated down i
  4. customThe residue was triturated with ether
  5. filtrationthe precipitate was filtered off
  6. washwashed with ether
  7. customdried in a HV

Quellen und Nachweise

ORD-Eintrag
ord-a804382e0dbb42df9fcaf6cef49aebde
Quelldatensatz
uspto-grants-2008_04
Patentnummer
US07351719B2

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