Reaktion #1007923

Reaktionsgleichung

Intermediate 226A

2-(3,3-Difluorocyclobutyl)-2-methylpropanenitrile

NaOH

ethanol

→

Intermediate 226B

Ausbeute 60.0%

2-(3,3-Difluorocyclobutyl)-2-methylpropanoic acid

Ausbeute 60.0%

Lösungsmittel

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction was then concentrated
2. 2
   Extraktionextracted with EtOAc (3×10 mL)
3. 3
   TrocknenThe combined organic layer was dried over Na2SO4
4. 4
   Filtrationfiltered
5. 5
   Sonstigethe filtrate evaporated under reduced pressure

Vorschrift

To a solution of Intermediate 226A (150 mg, 0.942 mmol) in ethanol (10 mL) and H2O (10 mL) was added a 10% aqueous solution of NaOH (10 mL, 0.942 mmol) and the reaction mixture was stirred at 90° C. for 12 h. The reaction was then concentrated and the pH of the resultant residue was adjusted to 4 with a 1.5 N aq. solution of HCl and then extracted with EtOAc (3×10 mL). The combined organic layer was dried over Na2SO4, filtered and the filtrate evaporated under reduced pressure to afford Intermediate 226B as a yellow sticky liquid (100 mg, 60%). 1H NMR (400 MHz, chloroform-d) δ ppm 12.30 (bs, 1H), 2.40-2.57 (m, 5H), 1.23 (s, 6H).

Quelle