Potassium thiocyanate → HCID 59386313, Verbindung

HRID 1969517Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1969517
[CH3:1][C:2]1([S:5]([O:8]CCCC)(=[O:7])=[O:6])[CH2:4][CH2:3]1.[S-]C#N.[K+:16]>O1CCOCC1.O>[CH3:1][C:2]1([S:5]([O-:8])(=[O:7])=[O:6])[CH2:4][CH2:3]1.[K+:16]

Komponenten

4

Edukt 2

HCID 516872Potassium thiocyanateHCID 58133073Butyl 1-methylcyclopropane-1-sulfonate

Produkt 1

HCID 59386313HCID 59386313, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 218864351,4-Dioxane--water (1/1)Lösungsmittel

Versuchsvorschrift

A mixture of butyl 1-methylcyclopropane-1-sulfonate (0.80 g, 4.2 mmol) and potassium thiocyanate (0.404 g, 4.16 mmol) in 1,4-dioxane/water (1:1, 10 mL) was heated at reflux for about 8 h. The reaction was cooled to ambient temperature and the solvents were concd under reduced pressure to yield crude potassium 1-methylcyclopropane-1-sulfonate which was suspended in thionyl chloride (7 mL). DMF (0.05 mL) was added and the mixture was heated at reflux for about 8 h and then cooled. The volatiles were removed under reduced pressure and the residue was dissolved in DCM (20 mL), washed with water (15 mL), dried over anhydrous MgSO4 and concd under reduced pressure to yield 1-methylcyclopropane-1-sulfonyl chloride (0.56 g, 86%) as a yellow oil. 1H NMR (DMSO-d6) δ 1.82 (br s, 2H), 1.79 (s, 3H), 1.15 (m, 2H).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for about 8 h

Quellen und Nachweise

ORD-Eintrag
ord-3f777f26663b4d41a3a4b5a11529ac69
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08426411B2

Notizen zur Reaktion

Wird geladen…