반응 #8896

반응 방정식

product

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

acetoxyacetyl chloride

acetonitrile

→

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

용매

ethyl acetate

반응 조건

후처리

1. 1
   세척washed two times with aqueous sodium bicarbonate
2. 2
   건조The organic layer was dried over sodium sulfate
3. 3
   농축then concentrated
4. 4
   기타The residue was triturated in 10 mL of methanol
5. 5
   기타The solid product was collected
6. 6
   세척rinsed two times with methanol
7. 7
   기타then dried in vacuo

실험 절차

The product of Step B (0.120 g; 0.253 mmol) and acetoxyacetyl chloride (0.11 mL; 1.01 mmol) were added to 2 mL of acetonitrile and stirred at room temperature. After 50 minutes the reaction mixture was diluted with ethyl acetate and washed two times with aqueous sodium bicarbonate. The organic layer was dried over sodium sulfate then concentrated. The residue was triturated in 10 mL of methanol. The solid product was collected and rinsed two times with methanol then dried in vacuo. HPLC/MS 576.8 (M+2); Rt=4.32 min.

출처