反応 #2267083

ord-b2fc670c69b2414b9437c45038c7b1c8

反応方程式

COc1cc(CCO)ccc1O
4-Hydroxy-3-methoxyphenethyl alcohol
CCCO
1-propanol
CCCOC(=O)Cc1ccc(O)c(OC)c1
15-A
CCCOC(=O)Cc1ccc(O)c(OC)c1
3-methoxy-4-hydroxyphenylacetic acid propyl ester

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the 1-propanol was removed under reduced pressure
  2. 2
    workup.ADDITIONthe resulting oil was diluted with ethyl acetate
  3. 3
    洗浄washed with saturated sodium bicarbonate solution
  4. 4
    workup.DISTILLATIONdistilled water
  5. 5
    乾燥The solution was dried over magnesium sulfate
  6. 6
    ろ過filtered
  7. 7
    その他the solvent was removed under reduced pressure

実験手順

4-Hydroxy-3-methoxyphenethyl alcohol (Sigma-Aldrich) was dissolved in anhydrous 1-propanol. To this solution ˜5 drops of concentrated sulphuric acid were added and the solution was heated at 100° C. for 3-5 hours in a pressure tube. When the reaction was complete, the 1-propanol was removed under reduced pressure, the resulting oil was diluted with ethyl acetate and washed with saturated sodium bicarbonate solution, distilled water, and then brine. The solution was dried over magnesium sulfate and filtered and the solvent was removed under reduced pressure, giving 15-A as a red oil in almost quantitative yield.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06887866B2uspto-grants-2005_05