Reaktion #640680

Reaktionsgleichung

1-methyl-1H-pyrazole

chlorosulfonic acid

→

1-Methyl-1H-pyrazole-4-sulfonyl chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturHeat
2. 2
   Sonstigereaction mixture at 110° C. for 3 hr
3. 3
   TemperaturCool to room temperature
4. 4
   workup.ADDITIONpour carefully
5. 5
   Sonstigeinto crushed ice
6. 6
   workup.STIRRINGwith stirring
7. 7
   SonstigeRecover the resulting white solid
8. 8
   Filtrationby vacuum filtration
9. 9
   Waschenwash with water
10. 10
    Sonstigedry under vacuum
11. 11
    Sonstigewithout further purification

Vorschrift

Add 1-methyl-1H-pyrazole (100 g, 1.18 mol) dropwise to chlorosulfonic acid (325 mL, 4.84 mol) stirring at 0° C. under nitrogen atmosphere. Heat reaction mixture at 110° C. for 3 hr. Cool to room temperature, then pour carefully into crushed ice with stirring. Recover the resulting white solid by vacuum filtration, wash with water, and dry under vacuum. Use the resulting material (72.2 g, 33%) without further purification.

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