Formaldehyde → HCID 23149182, Verbindung

HRID 1983055Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1983055
[Cl:1][C:2]([Cl:10])([F:9])[S:3][C:4]1[CH:5]=[N:6][NH:7][CH:8]=1.[O:11]1CCC[CH2:12]1.C=O>O.[OH-].C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:1][C:2]([Cl:10])([F:9])[S:3][C:4]1[CH:5]=[N:6][N:7]([CH2:12][OH:11])[CH:8]=1

Komponenten

6

Edukt 3

HCID 712FormaldehydeHCID 8028TetrahydrofuranHCID 23149183HCID 23149183, Verbindung

Produkt 1

HCID 23149182HCID 23149182, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel3×HCID 2723671Tetrabutylammonium HydroxideLösungsmittel

Versuchsvorschrift

0.19 g of 4-{[dichlorofluoromethyl]thio}-1H-pyrazole was dissolved to 5 ml of tetrahydrofuran. 5 ml of formaldehyde 36% in water and 0.1 ml of tetrabutylammonium hydroxide 10% in water were added to the solution, followed by stirring at room temperature for 4 hours. Water was added to the reaction mixture, and extracted with MTBE. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.22 g of 4-{[dichlorofluoromethyl]thio}-1H-pyrazole-1-ylmethanol.

Aufarbeitung

  1. extractionextracted with MTBE
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-88e67316c6b842e086de44ac8c9843c5
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07541374B2

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