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Methyl iodide → 7-Chloro-4-methyl-3-methylsulfanyl-4H-1,2,4-benzothiadiazine 1,1-dioxide

HRID 1066154
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1066154
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[NH:6][C:7]([S:12][CH3:13])=[N:8][S:9](=[O:11])(=[O:10])[C:4]=2[CH:3]=1.[C:16](=O)([O-])[O-].[K+].[K+].CI>C(#N)C.CO>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[N:6]([CH3:16])[C:7]([S:12][CH3:13])=[N:8][S:9](=[O:11])(=[O:10])[C:4]=2[CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 127001067-Chloro-3-(methylthio)-4H-benzo[e][1,2,4]thiadiazine 1,1-dioxide

Produkt 1

HCID 211978047-Chloro-4-methyl-3-methylsulfanyl-4H-1,2,4-benzothiadiazine 1,1-dioxide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel
HCID 6342
Acetonitrile
Lösungsmittel

Versuchsvorschrift

A solution of 7-chloro-3-methylsulfanyl-4H-1,2,4-benzothiadiazine 1,1-dioxide (0.8 g) in acetonitrile (24 mL) and methanol (0.5 mL) was supplemented with potassium carbonate (0.96 g), then with methyl iodide (3 mL), and stirred at room temperature for 10 h. The solvent was removed by distillation under reduced pressure. The residue was suspended in water (40 mL) and the pH was adjusted to pH 2 with formic acid. The precipitate of the title compound was collected by filtration, washed with water and dried. The compound was used without further purification in the next step (yield: 0.53 g).

Aufarbeitung

  1. customThe solvent was removed by distillation under reduced pressure
  2. filtrationThe precipitate of the title compound was collected by filtration
  3. washwashed with water
  4. customdried
  5. customThe compound was used without further purification in the next step (yield: 0.53 g)

Quellen und Nachweise

ORD-Eintrag
ord-11bd17b8349c44cca3c109fcea3c9034
Quelldatensatz
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06242443B1

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