反応 #8911

反応方程式

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

溶媒

CH2Cl2

acetonitrile

反応条件

後処理

1. 1
   洗浄washed two times with aqueous sodium bicarbonate
2. 2
   乾燥The organic layer was dried over sodium sulfate
3. 3
   濃縮then concentrated
4. 4
   その他was suspended in 150 mL of methanol at 60–65° C
5. 5
   温度After cooling to room temperature the methanol
6. 6
   その他was decanted away
7. 7
   洗浄the solid rinsed three times with fresh methanol
8. 8
   その他The solids were then dried in vacuo

実験手順

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.

出典