تفاعل #2487394

معادلة التفاعل

lithium aluminum hydride

2-hydroxynicotinic acid

→

3-hydroxymethyl-2-pyridone

المردود 32.4%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   أخرىreturned to room temperature
2. 2
   درجة الحرارةbefore being refluxed for 8 h
3. 3
   درجة الحرارةThe reaction was cooled to room temperature
4. 4
   أخرىwas quenched with 1.6 mL of water, 1.6 mL of 15% NaOH
5. 5
   أخرىThe solvent was removed in vacuo
6. 6
   ترشيحThe solution was filtered through celite
7. 7
   أخرىthe solvent removed in vacuo

الإجراء التجريبي

In Example 1, 1.6063 g (42.33 mmol) of lithium aluminum hydride (LAH) was suspended in 100 mL of tetrahydrofuran (THF) in a 250 mL round bottom flask (RBF) under the presence of argon gas (99.999% purity) and was cooled to 0° C. in an ice bath. 5.0946 g (36.62 mmol) of 2-hydroxynicotinic acid was slowly added, and the solution returned to room temperature before being refluxed for 8 h. The reaction was cooled to room temperature and was quenched with 1.6 mL of water, 1.6 mL of 15% NaOH and an additional 4.8 mL of water. The solvent was removed in vacuo and the residue was taken up in 100 mL of refluxing ethanol. The solution was filtered through celite and the solvent removed in vacuo to produce 1.4848 g (32.40% yield) of 3-hydroxymethyl-2-pyridone. Characterization data of the product was consistent with literature.

المصدر