反応 #1687646

反応方程式

4-acetoxy-2-fluorobenzoic acid

thionyl chloride

→

4-acetoxy-2-fluoro-1-(1-ethylpropyloxycarbonyl)benzene

反応条件

後処理

1. 1
   その他to react
2. 2
   温度under reflux for 5 hours
3. 3
   workup.DISTILLATIONThereafter, excessive thionyl chloride was distilled off
4. 4
   workup.ADDITIONa mixture comprising 1 ml of pyridine, 4 ml of dry ether and 0.6 g of 3-pentanol was added dropwise to the above mixture
5. 5
   workup.ADDITIONAfter the addition
6. 6
   workup.ADDITIONdiluted with 200 ml of ether
7. 7
   洗浄an organic layer was washed consecutively with diluted hydrochloric acid
8. 8
   乾燥a 1N sodium hydroxide aqueous solution and water, and dried over magnesium sulfate

実験手順

1.0 Gram of 4-acetoxy-2-fluorobenzoic acid was added to 7 ml of thionyl chloride, and the mixture was allowed to react under reflux for 5 hours. Thereafter, excessive thionyl chloride was distilled off, and a mixture comprising 1 ml of pyridine, 4 ml of dry ether and 0.6 g of 3-pentanol was added dropwise to the above mixture. After the addition, the resulting mixture was stirred at room temperature for one day and diluted with 200 ml of ether, and an organic layer was washed consecutively with diluted hydrochloric acid, a 1N sodium hydroxide aqueous solution and water, and dried over magnesium sulfate.

出典