Acetyl chloride → HCID 178469414, Verbindung

HRID 2177722Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2177722
C(Cl)(=O)C.[C:5]1([S:11]([CH2:14][C:15]2[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:19]([O:26][CH3:27])[C:18]([C:28]3[N:32](C4CCCCO4)[N:31]=[CH:30][CH:29]=3)=[CH:17][CH:16]=2)(=[O:13])=[O:12])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>CO>[C:5]1([S:11]([CH2:14][C:15]2[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:19]([O:26][CH3:27])[C:18]([C:28]3[CH:29]=[CH:30][NH:31][N:32]=3)=[CH:17][CH:16]=2)(=[O:13])=[O:12])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Komponenten

4

Versuchsvorschrift

Acetyl chloride (0.1 ml) was added to methanol (10 ml) cooled in ice and the resultant solution was added to ethyl 6-(benzenesulphonylmethyl)-2-methoxy-3-[1-(tetrahydropyran-2-yl)pyrazol-5-yl]benzoate (Intermediate 47, 0.05 g). The resultant mixture was stirred at room temperature for 1 hour then evaporated to dryness. The residue was treated with sodium bicarbonate (saturated aqueous solution) and extracted with DCM, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give ethyl 6-(benzenesulphonylmethyl)-2-methoxy-3-(3-pyrazolyl)benzoate (0.041 g) as a gum.

Aufarbeitung

  1. temperaturecooled in ice
  2. customthen evaporated to dryness
  3. additionThe residue was treated with sodium bicarbonate (saturated aqueous solution)
  4. extractionextracted with DCM
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-9fc4b3acbf2c4ef9b612f2b423b6ba4f
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09067905B2

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