Methanol → HCID 86745510, Verbindung

HRID 2371420Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2371420
[O:1]=[C:2]1[CH:7]([CH2:8][C:9]([OH:11])=[O:10])[S:6](=[O:13])(=[O:12])[C:5]2[S:14][C:15]([S:17](=[O:20])(=[O:19])[NH2:18])=[CH:16][C:4]=2[NH:3]1.S(=O)(=O)(O)O.[CH3:26]O>>[O:1]=[C:2]1[CH:7]([CH2:8][C:9]([O:11][CH3:26])=[O:10])[S:6](=[O:13])(=[O:12])[C:5]2[S:14][C:15]([S:17](=[O:20])(=[O:19])[NH2:18])=[CH:16][C:4]=2[NH:3]1

Komponenten

4

Versuchsvorschrift

A mixture of (2,3-dihydro-2,4,4-trioxo-6-sulfamoyl-1H-thieno-[2,3-b][1,4]thiazin-3-yl)acetic acid (5 g) and concentrated sulfuric acid (3 ml) in methanol (50 ml) was heated to reflux for 5 hours. The solvent was removed and the residue was treated with ice cold water. The resulting solid was collected, rinsed with additional cold water and dried at 50° C. to yield 4.05 g. Recrystallization from water gave methyl (2,3-dihydro-2,4,4-trioxo-6-sulfamoyl-1H-thieno-[2,3-b][1,4]thiazin-3-yl)acetate, mp 223°-225° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 5 hours
  3. customThe solvent was removed
  4. additionthe residue was treated with ice cold water
  5. customThe resulting solid was collected
  6. washrinsed with additional cold water
  7. customdried at 50° C.
  8. customto yield 4.05 g
  9. customRecrystallization from water

Quellen und Nachweise

ORD-Eintrag
ord-584c26b8131540b495e64e6260ac1c82
Quelldatensatz
uspto-grants-1992_03
Patentnummer
US05093332

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