Trifluoroacetic acid → (3-Chloro-benzyl)-(4-piperazin-1-yl-pyrimidin-2-yl)-amine, hydrochloride

To a solution of 4-[2-(3-chloro-benzylamino)-pyrimidin-4-yl]-piperazine-1-carboxylic acid tert-butyl ester (I-3a) (48.5 mg, 0.12 mmol) in CH2Cl2 (1 mL) was added trifluoroacetic acid (139 μL, 1.8 mmol). After stirring at room temperature for 3 h, the mixture was poured into 1N NaOH (10 mL) and extracted with CH2Cl2 (1×35 mL). The organic layer was washed with brine, dried and concentrated to afford the title compound as a free amine. The free amine in CH2Cl2 (1 mL) was added to 1 M HCl in ether (0.10 mL, 0.10 mmol). After stirring for 10 min at room temperature, the solution was concentrated in vacuo to yield the hydrochloride salt (3-A) (32.4 mg) as a yellow solid.

1. extractionextracted with CH2Cl2 (1×35 mL)
2. washThe organic layer was washed with brine
3. customdried
4. concentrationconcentrated

ORD-Eintrag

ord-df116bf338b445ffbc65ebd097245990

Quelldatensatz

uspto-grants-2004_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06825198B2