반응 #731281

반응 방정식

3-(4-fluorophenyl)-1-isopropyl-1H-indole

methyl 3,3-dimethoxypropionate

acetic acid

acetic acid

phosphorus oxychloride

→

methyl trans-3-[3-(4-fluorophenyl)-1-isopropyl-1H-indol-2-yl]acrylate

수율 93.0%

용매

water

반응 조건

후처리

1. 1
   기타a reaction
2. 2
   workup.ADDITIONwas added dropwise into the reaction liquid
3. 3
   여과the precipitated crystals were filtrated
4. 4
   세척The crystals were washed with 20 vol % aqueous methanol
5. 5
   기타dried

실험 절차

1.01 g of 3-(4-fluorophenyl)-1-isopropyl-1H-indole, 0.92 g of methyl 3,3-dimethoxypropionate, 0.72 mL of 90 wt % aqueous acetic acid (containing 4 mmol of water) and 6 mL of glacial acetic acid were mixed, then, 0.33 g of phosphorus oxychloride was added dropwise into the mixture at an inner temperature of 25° C., the added mixture was stirred for 9 hours at the same temperature to cause a reaction. After completion of the reaction, 16 mL of water was added dropwise into the reaction liquid, and the precipitated crystals were filtrated. The crystals were washed with 20 vol % aqueous methanol, then, dried to obtain 1.25 g of methyl trans-3-[3-(4-fluorophenyl)-1-isopropyl-1H-indol-2-yl]acrylate (yellow solid). Yield: 93%.

출처