反応 #160412

反応方程式

2-cyclohexanesulfonyl-2-methyl-propionic acid ethyl ester

lithium hydroxide monohydrate

→

2-cyclohexanesulfonyl-2-methyl-propionic acid

収率 95.7%

溶媒

water

THF water

反応条件

後処理

1. 1
   洗浄washed with DCM (2×15 mL)
2. 2
   温度The basic aqueous layer was cooled in an ice bath
3. 3
   抽出The acidic aqueous layer was extracted with DCM (3×20 mL)
4. 4
   洗浄The combined organic extracts were washed with brine
5. 5
   乾燥dried over Na2SO4
6. 6
   ろ過filtered

実験手順

To a solution of 3.47 g (13.2 mmol) of 2-cyclohexanesulfonyl-2-methyl-propionic acid ethyl ester in THF/water (4/1, 50 mL) were added 1.11 g (26.4 mmol) of lithium hydroxide monohydrate. The reaction was stirred at room temperature for 18 h. The reaction was further diluted with water (20 mL) and then washed with DCM (2×15 mL). The basic aqueous layer was cooled in an ice bath and then acidified with 1M aqueous HCl solution to pH 2. The acidic aqueous layer was extracted with DCM (3×20 mL). The combined organic extracts were washed with brine, dried over Na2SO4 and filtered. Concentration of the filtrate under reduced pressure afforded 2.96 g of 2-cyclohexanesulfonyl-2-methyl-propionic acid.

出典