تفاعل #2275702

معادلة التفاعل

4′-chloro-3-methoxy-biphenyl-4-carboxylic acid methyl ester

H2O

LiOH

→

desired product

المردود 91.0%

4′-chloro-3-methoxy-biphenyl-4-carboxylic acid

المردود 91.0%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe resulting suspension is heated
2. 2
   درجة الحرارةto reflux for 2 hours
3. 3
   درجة الحرارةThe reaction is cooled
4. 4
   تركيزconcentrated under reduced pressure
5. 5
   ترشيحthe resulting solid is collected by filtration
6. 6
   غسيلwashed with H2O
7. 7
   أخرىdried

الإجراء التجريبي

To a solution of 4′-chloro-3-methoxy-biphenyl-4-carboxylic acid methyl ester, 8, (0.615 g, 2.22 mmol) in THF (20 mL) and H2O (5 mL) at room temperature is added LiOH (0.932 g, 22.2 mmol). The resulting suspension is heated to reflux for 2 hours. The reaction is cooled and concentrated under reduced pressure. The crude product is acidified using conc. HCl and the resulting solid is collected by filtration washed with H2O and dried to afford 0.532 g (91%) of the desired product as a grey solid. 1H NMR (400 MHz, CDCl3) δ ppm 10.69 (1H, br s), 8.26 (1H, d, J=8.1 Hz), 7.53-7.58 (2H, m), 7.44-7.50 (2H, m), 7.33 (1H, dd, J=8.1, 1.6 Hz), 7.20 (1H, d, J=1.3 Hz), 4.17 (3H, s). HPLC-MS: m/z 263 [M+H]+.

المصدر