Trichloromethanethiol → 3-(trichloromethylthio)-1,2,3-benzoxathiazin-4-(3H)-one 2-oxide

HRID 329005

Reaktionsgleichung

Reaktionsgleichung von HRID 329005
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:4](=[O:11])[NH:3][S:2]1=[O:12].[Cl:13][C:14]([SH:17])([Cl:16])[Cl:15]>C(Cl)Cl>[Cl:13][C:14]([Cl:16])([Cl:15])[S:17][N:3]1[C:4](=[O:11])[C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[O:1][S:2]1=[O:12]

Komponenten

4

Edukt 2

HCID 6390TrichloromethanethiolHCID 122208292-Oxobenzo[e]oxathiazin-4-one

Produkt 1

HCID 214408713-(trichloromethylthio)-1,2,3-benzoxathiazin-4-(3H)-one 2-oxideAusbeute 40,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A 300-ml flask equipped with a stirrer and thermomether was charged with 5.0 g (0.03 mol) of 1,2,3-benzoxthiazin-4-(3H)-one 2-oxide, 5.3 g (0.03 mol) of perchloromethyl mercaptan, 3.1 g (0.03 mol) of thiethylamine and 150 ml of methylene chloride. The resulting mixture was stirred at ambient temperature for 1 hour. At the end of this time, the reaction mixture was filtered and washed 3 times with equal amounts of water. After drying, the solvent was removed by evaporation. The crude product was passed through a 250-g silica-gel column using hexane, 10% ether/hexane, and 20% ether/hexane, respectively. Evaporation gave 4 g of 3-(trichloromethylthio)-1,2,3-benzoxathiazin-4-(3H)-one 2-oxide having a melting point of 65°-67° C.

Aufarbeitung

  1. customA 300-ml flask equipped with a stirrer
  2. filtrationAt the end of this time, the reaction mixture was filtered
  3. washwashed 3 times with equal amounts of water
  4. customAfter drying
  5. customthe solvent was removed by evaporation
  6. customEvaporation

Quellen und Nachweise

ORD-Eintrag
ord-2aed3fc981ea458aa0648f96ade10e6d
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04018920

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