反応 #1973905

反応方程式

toluene

compound ( 16 )

trans-4-(4-Ethoxy-2,3-difluorophenyl)-cyclohexanecarboaldehyde

acetone

Jones reagent

→

4-ethoxy-2,3-difluoro-(trans-4-cyclohexyl)-carboxylic acid

溶媒

water

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred at 35° C. for 2 hours
2. 2
   温度After the reaction mixture had been cooled to 30° C.
3. 3
   workup.ADDITIONmixed with it
4. 4
   その他had separated into two phases of organic and aqueous phases
5. 5
   抽出the extraction into an organic phase
6. 6
   その他The resulting organic phase was separated
7. 7
   洗浄washed successively with water
8. 8
   乾燥an aqueous solution of sodium thiosulfate and water, and then dried over anhydrous magnesium sulfate

実験手順

The compound (16) (10.0 g) and acetone (50 ml) were mixed and the mixture was stirred at 35° C. for 30 minutes. Jones reagent (8N) (4.7 ml) was added to the mixture in the temperature range of 30 to 40° C. and the mixture was stirred at 35° C. for 2 hours. After the reaction mixture had been cooled to 30° C., toluene (200 ml) and water (200 ml) were added to the mixture and mixed with it. The mixture was then allowed to stand until it had separated into two phases of organic and aqueous phases, and the extraction into an organic phase was carried out. The resulting organic phase was separated, and washed successively with water, an aqueous solution of sodium thiosulfate and water, and then dried over anhydrous magnesium sulfate, giving 4-ethoxy-2,3-difluoro-(trans-4-cyclohexyl)-carboxylic acid (31) (8.8 g). The yield based on the compound (16) was 83.1%.

出典