تفاعل #544505

معادلة التفاعل

3,6 Dichloropyridine-2-carboxylic acid

morpholine

morpholine

→

3-chloro-6-morpholinyl-2-pyridine carboxylic acid

المردود 53.0%

المذيبات

DMA

N,N dimethylacetamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheating
2. 2
   workup.WAITcontinued for 40 hours
3. 3
   أخرىwas removed in the presence of toluene
4. 4
   workup.DISSOLUTIONThe residue was dissolved in water
5. 5
   استخلاصextracted with ether
6. 6
   أخرىto remove excess morpholine
7. 7
   استخلاصthe product extracted into ether
8. 8
   أخرىCrystallization from water
9. 9
   أخرىgave a white solid, 369 mg (53% yield)

الإجراء التجريبي

3,6 Dichloropyridine-2-carboxylic acid (0.55 g, 2.86 mmol), morpholine (1.37 g, 15.7 mmol) and N,N dimethylacetamide (1.37 mL) were combined and stirred for 24 h at 80° C. An additional volume of morpholine (1.39 g, 15.7 mmol) was added and heating continued for 40 hours more. After cooling the DMA was removed in the presence of toluene. The residue was dissolved in water and extracted with ether to remove excess morpholine. The aqueous was acidified to pH=2 and the product extracted into ether. Crystallization from water gave a white solid, 369 mg (53% yield). 1H NMR (CD3OD): δ 3.52 (t, 4H), 3.78 (t, 4H), 6.97 (d,1H), 7.65 (d, 1H). LC-MS, M+H: 243.

المصدر