Acetyl chloride → HCID 18538875, Verbindung

1-Acetyl-N-{3-[4-(4-aminobenzyl)-1-piperidinyl]propyl}-N-(3,4-dichlorophenyl}-4-piperidinecarboxamide (Example 303) (18 mg, 6.033 mmol) was dissolved in tetrahydrofuran (0.3 mL). To the solution were added triethylamine (5.0 mg, 0.050 mmol) and acetyl chloride (3.4 mg, 0.043 mmol), and the mixture was stirred at room temperature for 30 minutes. To the reaction mixture was added aqueous solution of 1N-sodium hydroxide (5 mL), and the mixture was extracted with ethyl acetate (5 mL×2). The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The concentrate was subjected to alumina column chromatography (alumina 2 g, ethyl acetate), and the desired fraction was concentrated under reduced pressure to give the titled compound (18 mg, 0.031 mmol, Yield 93%) as a colorless oily substance.

1. extractionthe mixture was extracted with ethyl acetate (5 mL×2)
2. dry with materialThe organic layer was dried over magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. concentrationthe desired fraction was concentrated under reduced pressure

ORD-Eintrag

ord-bb96862d3a724033ab753ae78e9b41b9

Quelldatensatz

uspto-grants-2003_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06562978B1