Sodium Sulfite → 1,2-Benzisoxazole-3-methanesulfonate sodium

HRID 427087Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 427087
Br[CH2:2][C:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][N:4]=1.[S:12]([O-:15])([O-:14])=[O:13].[Na+:16].[Na+]>CO.O>[O:5]1[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[C:3]([CH2:2][S:12]([O-:15])(=[O:14])=[O:13])=[N:4]1.[Na+:16]

Komponenten

5

Edukt 2

HCID 24437Sodium SulfiteHCID 34991891,2-Benzisoxazole, 3-(bromomethyl)-

Produkt 1

HCID 236749341,2-Benzisoxazole-3-methanesulfonate sodium

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of 8.0 of 3-bromomethyl-1,2-benzisoxazole (m.p. 64°-66° C.) in 130 ml of methanol was added a solution of 8.1 g of sodium sulfite in 130 ml of water. The mixture was heated with stirring at 50° C. for 4 hours and concentrated under reduced pressure. The crystalline residue was dissolved in 250 ml of methanol with warming and the insoluble material was filtered off. The filtrate was concentrated under reduced pressure and the crystalline residue was washed with diethyl ether to give crude sodium 1,2-benzisoxazole-3-methanesulfonate (10.5 g).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe crystalline residue was dissolved in 250 ml of methanol
  4. temperaturewith warming
  5. filtrationthe insoluble material was filtered off
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. washthe crystalline residue was washed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-4386bd42a4e84c10953765be27bc669c
Quelldatensatz
uspto-grants-1979_10
Patentnummer
US04172896

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