تفاعل #42281

معادلة التفاعل

Lithium hydroxide monohydrate

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

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title compound

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

المذيبات

THF methanol water

water

hydrochloric acid

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONis added
2. 2
   استخلاصThe aqueous mixture is extracted with ethyl acetate
3. 3
   أخرىThe organic phase is separated
4. 4
   غسيلwashed with saline
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated

الإجراء التجريبي

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.

المصدر