Chloroform → 4-chloro-N-methylbenzothiazolone

HRID 847802

Reaktionsgleichung

Reaktionsgleichung von HRID 847802
[Cl:1][C:2]1[C:7]2[N:8]=[C:9](OC)S[C:6]=2[CH:5]=[CH:4][CH:3]=1.[S:13]([O:18]C)(OC)(=O)=O.[CH:20](Cl)(Cl)Cl>>[Cl:1][C:2]1[C:7]2[N:8]([CH3:9])[CH2:20][S:13](=[O:18])[C:6]=2[CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 3

HCID 6212ChloroformHCID 6497Dimethyl SulfateHCID 41419694-Chloro-2-methoxybenzothiazole

Produkt 1

HCID 696450104-chloro-N-methylbenzothiazoloneAusbeute 99,7 %

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A mixture of 4-chloro-2-methoxybenzothiazole (3.00 g, 0.015 mole) and dimethyl sulfate (95 mg, 7.5×10-4 mole) was heated at 150° C. for 3 hours with stirring. After cooling, the reaction mass was dissolved in chloroform, and the chloroform layer was washed with an aqueous solution saturated with sodium carbonate and then with water. The solvent was removed under reduced pressure to obtain 2.99 g of 4-chloro-N-methylbenzothiazolone as white crystals. Yield 99.7%, purity 99.0%, m.p. 130°-132° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. washthe chloroform layer was washed with an aqueous solution saturated with sodium carbonate
  3. customThe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-3430b6b0385643a59c87c7ea15694002
Quelldatensatz
uspto-grants-1981_10
Patentnummer
US04293702

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