反応 #347384

反応方程式

product

Valproic acid chloride

2-iodoethanol

→

valproic acid

収率 138.7%

反応条件

後処理

1. 1
   温度cooling in an ice bath
2. 2
   その他removed from the
3. 3
   温度heat
4. 4
   workup.STIRRINGstirred for an additional 10 minutes
5. 5
   workup.DISSOLUTIONThe reaction mixture was then dissolved in 50 ml of ether
6. 6
   洗浄washed with water (1×30 ml), 5% NaOH (2×30 ml)
7. 7
   乾燥The ether layer was dried over anhydrous sodium sulfate
8. 8
   その他the solvent was removed under reduced pressure

実験手順

To the product of Example 87 (4.87 g, 30 mmol), 2-iodoethanol (5.16 g, 30 mmol) was added with stirring and cooling in an ice bath. The neat mixture was then heated to 100° C. in a water bath for 10 minutes, then removed from the heat and stirred for an additional 10 minutes. The reaction mixture was then dissolved in 50 ml of ether, washed with water (1×30 ml), 5% NaOH (2×30 ml), and again with water (2×30 ml). The ether layer was dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure. A light yellow liquid product was obtained in 67% yield from valproic acid (6.0 g). Silver nitrate gave a bright yellow precipitate. NMR analysis confirmed the identity of the product.

出典