Reaktion #8911

Reaktionsgleichung

product

1-[3-Amino-6-(2-chlorophenyl)-5-(4-chlorophenyl)furo[2,3-b]pyridin-2-yl]-2-hydroxy-2-methylpropan-1-one

acetoxy acetylchloride

→

title compound

2-{[6-(2-Chlorophenyl)-5-(4-chlorophenyl)-2-(2-hydroxy-2-methylpropanoyl)furo[2,3-b]pyridin-3yl]amino}-2-oxoethyl acetate

Lösungsmittel

CH2Cl2

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed two times with aqueous sodium bicarbonate
2. 2
   TrocknenThe organic layer was dried over sodium sulfate
3. 3
   Einengenthen concentrated
4. 4
   Sonstigewas suspended in 150 mL of methanol at 60–65° C
5. 5
   TemperaturAfter cooling to room temperature the methanol
6. 6
   Sonstigewas decanted away
7. 7
   Waschenthe solid rinsed three times with fresh methanol
8. 8
   SonstigeThe solids were then dried in vacuo

Vorschrift

To a solution of 4.0 g of the product of Example 100 in 25 mL of acetonitrile was added 7.5 mL acetoxy acetylchloride and the reaction mixture was stirred at room temperature. After 50 min the reaction mixture was diluted with CH2Cl2 and washed two times with aqueous sodium bicarbonate. The organic layer was dried over sodium sulfate then concentrated. The residue was suspended in 150 mL of methanol at 60–65° C. After cooling to room temperature the methanol was decanted away and the solid rinsed three times with fresh methanol. The solids were then dried in vacuo to afford the title compound. HPLC/MS: 540.9 (M+1), 542.8 (M+3); Rt=4.07 min.

Quelle