تفاعل #2045105

معادلة التفاعل

Formaldehyde

benzamide

morpholine

→

Mannich base

المردود 30.0%

N-Morpholin-4-ylmethyl-benzamide

المردود 30.0%

المذيبات

MeOH

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe resulting solution was cooled in an ice bath
2. 2
   workup.WAITto stand at RT for another 10 min
3. 3
   أخرىwas placed in a 70° C.
4. 4
   أخرىfor 2 h
5. 5
   أخرىThe solvents were evaporated
6. 6
   أخرىthe isolated residue (a waxy solid) was chromatographed on a Chromatotron with dichloromethane/methanol mixture, 5:0.2 to 5:0.6 as eluent
7. 7
   أخرىThe desired fractions were collected
8. 8
   أخرىthe solvents were evaporated

الإجراء التجريبي

To a stirred solution of benzamide (0.30 g, 2.5 mmol) in MeOH (5 mL) was added morpholine (0.22 g, 2.5 mmol) and the resulting solution was cooled in an ice bath. Formaldehyde (0.215 mL, 2.5 mmol, 37% in water) was then added and the stirred solution was left on ice for 5 min and then it was allowed to stand at RT for another 10 min, and then it was placed in a 70° C. oil bath for 2 h. The solvents were evaporated and the isolated residue (a waxy solid) was chromatographed on a Chromatotron with dichloromethane/methanol mixture, 5:0.2 to 5:0.6 as eluent. The desired fractions were collected and the solvents were evaporated giving Mannich base 18 (0.145 g, 30%) as an oil which solidified in the freezer.

المصدر