تفاعل #5508

معادلة التفاعل

hydrochloric acid

Piperidine

2-oxo-1-azacyclotetradecane-3,14-dicarboxylic acid

paraformaldehyde

→

3-methylidene-2-oxo-1-azacyclotetradecane-14-carboxylic acid

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction is then cooled to 0° C.
2. 2
   أخرىThe reaction is partitioned between ethyl acetate and water
3. 3
   استخلاصthe aqueous phase is extracted several times with ethyl acetate
4. 4
   تجفيفThe combined organic layers are dried (Na2SO4)
5. 5
   أخرىthe solvent is evaporated

الإجراء التجريبي

2-oxo-1-azacyclotetradecane-3,14-dicarboxylic acid (0.868 g, 2.9 mmol) is dissolved in pyridine (15.0 mL). Piperidine (0.060 mL, 0.59 mmol) is added, followed by paraformaldehyde (0.133 g, 4.43 mmol), and the reaction is heated to 65° C. for 4 hours. The reaction is then cooled to 0° C., and concentrated hydrochloric acid is added to bring the pH to approximately 2. The reaction is partitioned between ethyl acetate and water, and the aqueous phase is extracted several times with ethyl acetate. The combined organic layers are dried (Na2SO4), and the solvent is evaporated to give 3-methylidene-2-oxo-1-azacyclotetradecane-14-carboxylic acid.

المصدر