Реакция #8911

Уравнение реакции

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

Растворители

CH2Cl2

acetonitrile

Условия реакции

Обработка

1. 1
   Промывкаwashed two times with aqueous sodium bicarbonate
2. 2
   СушкаThe organic layer was dried over sodium sulfate
3. 3
   Концентрированиеthen concentrated
4. 4
   Другоеwas suspended in 150 mL of methanol at 60–65° C
5. 5
   ТемператураAfter cooling to room temperature the methanol
6. 6
   Другоеwas decanted away
7. 7
   Промывкаthe solid rinsed three times with fresh methanol
8. 8
   ДругоеThe solids were then dried in vacuo

Методика

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.

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