Diisopropylethylamine → HCID 58378949, compound

Participants

Reaction Conditions

Reaction Steps

Add 1-chloro-4-(4-fluorophenyl)phthalazine (200 g, 773 mmol) to a solution of (S)-tert-butyl 3-methylpiperazine-1-carboxylate (232 g, 1.16 mol), diisopropylethylamine (674 mL, 28.1 mol), and DMSO (2.0 L). Heat the mixture to 120° C. for 60 h. Cool the mixture to 25° C., pour into ice water (3.0 L) and filter. Collect the solids, dissolve in CH2Cl2 (2.0 L), and extract with water (2.0 L). Concentrate the organic phase and add to a silica plug (3.0 kg silica) eluting with 3% THF in CH2Cl2 to yield the title compound as a yellow foam (126 g, 38%). ES/MS m/z 423.0 (M+1).

Provenance & Evidence