N-Methylbenzylamine → N-Benzyl-3-[4-(3,3-diphenyl-1-propyl)piperazin-1-yl]-N-methylbenzamide

The compound (0.10 g) prepared in step (c) was dissolved in dichloromethane (2 ml). A BOP reagent (0.10 g) and diisopropylethylamine (0.052 ml) were added to the solution. The mixture was stirred at room temperature for 30 min. N-Methylbenzylamine (0.039 ml) was then added thereto, and the mixture was stirred at room temperature overnight. The reaction solution was extracted with ethyl acetate, followed by washing with water. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was then removed by distillation under the reduced pressure. The residue was purified by preparative TLC (hexane:ethyl acetate=1:1) to give 0.072 g (57.3%) of the title compound.

1. stirringthe mixture was stirred at room temperature overnight
2. extractionThe reaction solution was extracted with ethyl acetate
3. washby washing with water
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. customthe solvent was then removed by distillation under the reduced pressure
6. customThe residue was purified by preparative TLC (hexane:ethyl acetate=1:1)

ORD-Eintrag

ord-f4b5b500353a41b1bbd0aaebbaf428c5

Quelldatensatz

uspto-grants-2004_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06777414B1