p-Toluenesulfonic acid monohydrate → HCID 86612133, Verbindung

HRID 1162310Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1162310
[CH3:1][O:2][C:3]([CH:6]1[CH2:10][O:9]C(C)(C)[N:7]1[C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])([CH3:5])[CH3:4].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[OH:9][CH2:10][CH:6]([NH:7][C:13](=[O:14])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[C:3]([O:2][CH3:1])([CH3:4])[CH3:5]

Komponenten

4

Edukt 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 23138231Tert-butyl 4-(1-methoxy-1-methylethyl)-2,2-dimethyl-1,3-oxazolidine-3-carboxylate

Produkt 1

HCID 86612133HCID 86612133, VerbindungAusbeute 98,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

tert-Butyl 4-(1-methoxy-1-methylethyl)-2,2-dimethyl-1,3-oxazolidine-3-carboxylate (2.5 g) obtained in Example 73a) was dissolved in methanol (45 ml), p-toluenesulfonic acid monohydrate (0.18 g) was added thereto, and mixed at room temperature for 20 minutes. The solvent was distilled off under reduced pressure, and the residue was diluted with ethyl acetate, washed with a saturated aqueous sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound as a colorless solid (2.1 g, 95%).

Aufarbeitung

  1. additionmixed at room temperature for 20 minutes
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionthe residue was diluted with ethyl acetate
  4. washwashed with a saturated aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b1926e87430e40ffae6ceeffc6bc2fa6
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07820673B2

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