تفاعل #1797257

معادلة التفاعل

3-[3-(Piperidinomethyl)phenoxy]propylamine

2,3-dichloropyridine

→

title compound

المردود 37.2%

2-[3-[3-(Piperidinomethyl)phenoxy]propylamino]-3-chloropyridine

المردود 37.2%

المذيبات

3-methylpyridine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 16 hours
2. 2
   أخرىThe majority of the reaction solvent was removed by vacuum distillation (120 torr, 70°-80° C.)
3. 3
   غسيلwashed with water (2×100 ml)
4. 4
   استخلاصextracted into chloroform (40 ml)
5. 5
   استخلاصThe chloroform extract
6. 6
   أخرىwas evaporated under reduced pressure

الإجراء التجريبي

3-[3-(Piperidinomethyl)phenoxy]propylamine (2.17 g) and 2,3-dichloropyridine (1.27 g) were dissolved in 3-methylpyridine (6 ml) and stirred under reflux for 16 hours. The majority of the reaction solvent was removed by vacuum distillation (120 torr, 70°-80° C.) and the residue was neutralised with aqueous potassium carbonate (5%; 40 ml), washed with water (2×100 ml) and extracted into chloroform (40 ml). The chloroform extract was evaporated under reduced pressure and subjected to column chromatography (chloroform:methanol 25:1) to give the title compound as an oil (1.15 g). This was treated with oxalic acid as in Example 1 to give 2-[3-[3-(piperidinomethyl)phenoxy]propylamino]-3-chloropyridine dioxalate (1.1 g), m.p. 154°-5° C.

المصدر