تفاعل #8911

معادلة التفاعل

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

المذيبات

CH2Cl2

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed two times with aqueous sodium bicarbonate
2. 2
   تجفيفThe organic layer was dried over sodium sulfate
3. 3
   تركيزthen concentrated
4. 4
   أخرىwas suspended in 150 mL of methanol at 60–65° C
5. 5
   درجة الحرارةAfter cooling to room temperature the methanol
6. 6
   أخرىwas decanted away
7. 7
   غسيلthe solid rinsed three times with fresh methanol
8. 8
   أخرىThe solids were then dried in vacuo

الإجراء التجريبي

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.

المصدر