1-(4-Fluorophenyl)piperazine → HCID 59833503, Verbindung

2-(1H-Benzotriazol-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (150 mg, 0.47 mmol), diisopropylethylamine (102 mg, 0.8 mmol) and 1-(4-fluorophenyl)piperazine (65 mg, 0.47 mmol) were added sequentially at ambient temperature to a stirred solution of 3-(4-oxo-3,4-dihydrophthalazin-1-ylmethyl)benzoic acid (A) (100 mg, 0.36 mmol) in dry dimethylacetamide (1 ml), the mixture was stirred at ambient temperature for 4 hours and allowed to stand at ambient temperature for 16 hours, then it was added dropwise to stirred cold water (10 ml). After 30 minutes, the resulting solid was collected by filtration, washed with water (2×1 ml) and hexane (1 ml), dried in vacuo and purified using preparative HPLC to give 4-{3-[4-(4-fluorophenyl)piperazin-1-ylcarbonyl]benzyl}-1(2H)-phthalazinone (21) (76 mg) as a cream solid; m/z (M+H)+• 443; HPLC Purity 90%; HPLC Retention time 4.00 minutes.

1. waitto stand at ambient temperature for 16 hours
2. additionit was added dropwise
3. waitAfter 30 minutes
4. filtrationthe resulting solid was collected by filtration
5. washwashed with water (2×1 ml) and hexane (1 ml)
6. customdried in vacuo
7. custompurified

ORD-Eintrag

ord-7a58d40342674a34a9d16d4f6426c355

Quelldatensatz

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07981889B2