HCID 18353297, Verbindung → Methyl 2-(m-methylbenzylthio)-5-trifluoromethylbenzoate

HRID 978087Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 978087
[CH3:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][CH:22]=1)[CH2:5][S:6][C:7]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][C:8]=1[C:9]([OH:11])=[O:10].NO[C:25]1CCCCCC=1>C(OCC)C>[CH3:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][CH:22]=1)[CH2:5][S:6][C:7]1[CH:15]=[CH:14][C:13]([C:16]([F:17])([F:18])[F:19])=[CH:12][C:8]=1[C:9]([O:11][CH3:25])=[O:10]

Komponenten

4

Edukt 2

HCID 18353297HCID 18353297, VerbindungHCID 202050722-(m-Methylbenzylthio)-5-trifluoromethylbenzoic acid

Produkt 1

HCID 13787728Methyl 2-(m-methylbenzylthio)-5-trifluoromethylbenzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A mixture of 2-(m-methylbenzylthio)-5-trifluoromethylbenzoic acid (1.65 g, 5.06 mmol) and 1-aza-2-methoxy-1-cycloheptene (643 mg, 5.06 mmol) was heated at 80°-85° C. for 18 hours, cooled, diluted with diethyl ether, washed with 1N aqueous sodium hydroxide solution, water, dried (sodium sulfate), and evaporated. The product was crystallized from methanol; yield 885 mg (51%). The 60 MHz NMR spectrum in chloroform-d was in accord with the desired structure.

Aufarbeitung

  1. temperaturewas heated at 80°-85° C. for 18 hours
  2. temperaturecooled
  3. washwashed with 1N aqueous sodium hydroxide solution, water
  4. dry with materialdried (sodium sulfate)
  5. customevaporated
  6. customThe product was crystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-a03ea212e42c44d9a79ad93b0a770a3e
Quelldatensatz
uspto-grants-1987_05
Patentnummer
US04663344

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