2-(4-Morpholino)thiobenzothiazole → 2-Morpholinosulphinyl-benzothiazole

HRID 328328

Reaktionsgleichung

Reaktionsgleichung von HRID 328328
[O:1]1[CH2:6][CH2:5][N:4]([S:7][C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)[CH2:3][CH2:2]1.C(=O)([O-])[O-:18].[Na+].[Na+].C(=O)(O)[O-].[Na+].Cl[O-].[Na+].[OH-].[Na+]>O>[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[O:18])[CH2:3][CH2:2]1

Komponenten

7

Edukt 5

HCID 76192-(4-Morpholino)thiobenzothiazoleHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 23665760Sodium Hypochlorite2×

Produkt 1

HCID 6678152-Morpholinosulphinyl-benzothiazoleAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

37.8 parts of 2-morpholinosulphenyl-benzothiazole are suspended in 65 parts of water containing 5 parts of sodium carbonate and 1 part of sodium bicarbonate. 90 parts by volume of an aqueous solution of sodium hypochlorite titrating 177 g. of NaClO and 3 g. of free caustic soda per liter are slowly introduced in a period of one hour into the well stirred suspension. The temperature is maintained at 25° C. and the mixture is stirred for 20 hours at this temperature. It is filtered, the solid is washed until neutral and dried under vacuum. 37 parts of 2-morpholinosulphinyl-benzothiazole melting at 93°-94° C. are obtained, that is a yield of 93%. On recrystallisation from a benzene/petrol ether mixture, the melting point is 99° C. (uncorrected).

Aufarbeitung

  1. stirringthe mixture is stirred for 20 hours at this temperature
  2. filtrationIt is filtered
  3. washthe solid is washed until neutral and
  4. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-0dd844f0b9774f239f62927bf6b30e8c
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04017506

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