Anisole → HCID 178521930, Verbindung

HRID 132062

Reaktionsgleichung

Reaktionsgleichung von HRID 132062
[C:1]1([NH:7][C:8]([C:10]2[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([CH2:21][OH:22])[CH:16]=3)=[CH:13][N:12](CC3C=CC(OC)=CC=3)[N:11]=2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(OC)C=CC=CC=1>FC(F)(F)C(O)=O>[C:1]1([NH:7][C:8]([C:10]2[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([CH2:21][OH:22])[CH:16]=3)=[CH:13][NH:12][N:11]=2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 7519AnisoleHCID 668554221h-Pyrazole-3-carboxamide,4-[3-(hydroxymethyl)phenyl]-1-[(4-methoxyphenyl)methyl]-n-phenyl-

Produkt 1

HCID 178521930HCID 178521930, VerbindungAusbeute 35,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 4-(3-hydroxymethyl-phenyl)-1-(4-methoxy-benzyl)-1H-pyrazole-3-carboxylic acid phenylamide (20 mg) and anisole (20 μl) in trifluoroacetic acid (1 ml) was heated at 120° C. (50 W) for 15 minutes in a CEM Discover microwave synthesiser. The reaction was evaporated then purified by flash column chromatography eluting with 2:1 ethyl acetate/hexane. Product containing fractions were combined and evaporated to give 5 mg of product. (LC/MS: Rt 2.55 [M+H]+294).

Aufarbeitung

  1. customThe reaction was evaporated
  2. customthen purified by flash column chromatography
  3. washeluting with 2:1 ethyl acetate/hexane
  4. additionProduct containing fractions
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-685b1dd45da14f468377f574b50c1337
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07385059B2

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