反応 #82113

反応方程式

Ferulic acid

n-propyl alcohol

hydrogen chloride

→

compound

収率 91.6%

n-propyl ferulate

収率 91.6%

溶媒

n-hexane ethyl acetate

反応条件

後処理

1. 1
   その他were placed in an egg-plant type flask
2. 2
   温度(200 ml), and heated
3. 3
   温度under reflux overnight
4. 4
   その他the solvent was evaporated under reduced pressure by a rotary evaporator
5. 5
   workup.ADDITIONBenzene was added to the residue
6. 6
   その他the solvent was again evaporated by a rotary evaporator
7. 7
   その他to obtain the crude product
8. 8
   その他The resulting crude product was separated
9. 9
   その他purified by silica gel column chromatography (diameter=5.5×7.0 cm; 60 g; n-hexane/ethyl acetate=2/1)

実験手順

Ferulic acid (4.85 g) and then n-propyl alcohol (50 ml) containing hydrogen chloride (4%) were placed in an egg-plant type flask (200 ml), and heated under reflux overnight. The disappearance of the starting material was confirmed by thin layer chromatography (TLC: n-hexane/ethyl acetate=2/1), then the solvent was evaporated under reduced pressure by a rotary evaporator. Benzene was added to the residue, and then, the solvent was again evaporated by a rotary evaporator to obtain the crude product. The resulting crude product was separated and purified by silica gel column chromatography (diameter=5.5×7.0 cm; 60 g; n-hexane/ethyl acetate=2/1) to obtain the above-identified compound (5.48 g, 91.6%) as colorless oil.

出典