Reaktion #1568291

Reaktionsgleichung

3-{[7-(2-chloro-4-fluoro-phenoxy)-1-cyano-4-hydroxy-isoquinoline-3-carbonyl]-amino}-2,2-dimethyl-propionic acid tert-butyl ester

→

title compound

Ausbeute 68.1%

3-{[7-(2-Chloro-4-fluoro-phenoxy)-1-cyano-4-hydroxy-isoquinoline-3-carbonyl]amino}-2,2-dimethyl-propionic acid

Ausbeute 68.1%

Lösungsmittel

TFA CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeReaction mixture
2. 2
   Einengenwas concentrated
3. 3
   workup.DISSOLUTIONThe residue was dissolved in water (30 mL)
4. 4
   SonstigePrecipitate was collected
5. 5
   Waschenrinsed with water
6. 6
   Sonstigedried in vacuo

Vorschrift

A mixture of 3-{[7-(2-chloro-4-fluoro-phenoxy)-1-cyano-4-hydroxy-isoquinoline-3-carbonyl]-amino}-2,2-dimethyl-propionic acid tert-butyl ester (40 mg, 0.08) in (½) TFA/CH2Cl2 (3 mL) was stirred at room temperature for 4 h. Reaction mixture was concentrated. The residue was dissolved in water (30 mL) and the pH was adjusted to 10 by 1 N NaOH. It was then acidified by 1 N HCl to pH=3-4. Precipitate was collected, rinsed with water and dried in vacuo to provide the title compound 24 mg (0.053 mmol) in 66% yield. LC-MS ESI−: 456.05 (M−1)−.

Quelle