반응 #1812502

반응 방정식

ethyl acetate

( 7 )

2-{4-[4-(2-hydroxy-ethylsulfanyl}-phenylsulfanyl]-phenylsulfanyl}-ethanol

diisopropylethylamine

acryloyl chloride

→

( 8 )

acrylic acid 2-{4-[4-(2-acryloyloxy-ethylsulfanyl) -phenylsulfanyl]-phenylsulfanyl}-ethyl ester

반응 조건

후처리

1. 1
   workup.ADDITIONwas poured into a mixture
2. 2
   workup.STIRRINGAfter stirring for five minutes the organic phase
3. 3
   기타was removed
4. 4
   세척washed with saturated KCl solution
5. 5
   기타The solvent was removed
6. 6
   기타the residue purified on column chromatography (silica gel eluted with 25% ethylacetate/hexane)

실험 절차

A solution containing 13 grams of (7) and 14.9 grams of diisopropylethylamine was cooled to 5° C., and to it was added 10.4 grams of acryloyl chloride over a period of 20 minutes. The mixture was stirred at 5-10° C. for two hours after which it was poured into a mixture containing 75 ml of 1N HCL and 100 ml of ethyl acetate. After stirring for five minutes the organic phase was removed and washed with saturated KCl solution followed by 10 percent aqueous potassium bicarbonate. The solvent was removed and the residue purified on column chromatography (silica gel eluted with 25% ethylacetate/hexane) to yield in the first fraction 8.5 grams of (8).

출처