Methanol → 2-(4-Acetylphenylsulfonamido)-2-methylpropionic acid

HRID 1519107

Reaktionsgleichung

Reaktionsgleichung von HRID 1519107
C[O:2][C:3](=[O:20])[C:4]([NH:7][S:8]([C:11]1[CH:16]=[CH:15][C:14]([C:17](=[O:19])[CH3:18])=[CH:13][CH:12]=1)(=[O:10])=[O:9])([CH3:6])[CH3:5].C1COCC1.CO.O[Li].O>O>[C:17]([C:14]1[CH:15]=[CH:16][C:11]([S:8]([NH:7][C:4]([CH3:6])([CH3:5])[C:3]([OH:20])=[O:2])(=[O:10])=[O:9])=[CH:12][CH:13]=1)(=[O:19])[CH3:18]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 60744560Methyl-2-(4-acetylphenylsulfonamido)-2-methylpropanoate

Produkt 1

HCID 210825082-(4-Acetylphenylsulfonamido)-2-methylpropionic acidAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

methyl-2-(4-acetylphenylsulfonamido)-2-methylpropanoate (2.55 g, 8.52 mmol) was charged, and dissolved through addition of THF (20 ml), and methanol (20 ml). LiOH.H2O dissolved in H2O (10 ml) was added thereto, followed by stirring for 12 hours at room temperature. After stirring for 12 hours, the resultant solution was vacuum-evaporated, acidified with 2N—HCl to pH 2-3, and extracted with EA (×2). The organic layer was dried with MgSO4, and filtered. Through vacuum distillation, the solvent was removed so as to obtain 2-(4-acetylphenylsulfonamido)-2-methylpropionic acid (2.38 g, 8.35 mmol, 98%).

Aufarbeitung

  1. additionwas added
  2. stirringAfter stirring for 12 hours
  3. customthe resultant solution was vacuum-evaporated
  4. extractionextracted with EA (×2)
  5. dry with materialThe organic layer was dried with MgSO4
  6. filtrationfiltered
  7. distillationThrough vacuum distillation
  8. customthe solvent was removed so as

Quellen und Nachweise

ORD-Eintrag
ord-2e9a62c457ff4e29bbd5ffbaecb32443
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073830B2

Verknüpfte Notizen

Wird geladen…