反応 #42281

反応方程式

Lithium hydroxide monohydrate

methyl 3-[(dipropylamino)carbonyl]-5-ethylbenzoate

→

title compound

3-[(Dipropylamino)carbonyl]-5-ethylbenzoic acid

溶媒

THF methanol water

water

hydrochloric acid

反応条件

後処理

1. 1
   workup.ADDITIONis added
2. 2
   抽出The aqueous mixture is extracted with ethyl acetate
3. 3
   その他The organic phase is separated
4. 4
   洗浄washed with saline
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   ろ過filtered
7. 7
   濃縮concentrated

実験手順

Lithium hydroxide monohydrate (0.0680 g, 1.6 mmol) is added to a mixture of methyl 3-[(dipropylamino)carbonyl]-5-ethylbenzoate (PREPARATION 20, 0.450 g, 1.6 mmol) in a mixture of THF/methanol/water (2/1/1, 8 mL). The mixture is stirred at 20-25 degrees C. for 3 hours. The mixture is then diluted with water (20 mL) and hydrochloric acid (1 N) is added to bring the pH to less than 3. The aqueous mixture is extracted with ethyl acetate. The organic phase is separated and washed with saline, dried over anhydrous magnesium sulfate, filtered and concentrated to give the title compound, MS (ESI+) for C16H23NO3 m/z (M+H)+=278.2.

出典