Trifluoroacetic acid → 5-Bromo-3-nitro-4-(4-(pyrimidin-5-ylmethyl)piperazin-1-yl)pyridin-2-amine

This was prepared using the same procedure as for 5-bromo-3-nitro-4-(4-(1-(pyridin-2-yl)ethyl)piperazin-1-yl)pyridin-2-amine, but here using tert-butyl 4-(pyrimidin-5-ylmethyl)piperazine-1-carboxylate (1.1 eq, 0.37 mmol, 104 mg), TFA (1.5 mL) and CH2Cl2 (4 mL), then 5-bromo-4-chloro-3-nitropyridin-2-amine (86 mg, 0.34 mmol) in iPrOH (3 mL) and DIPEA (0.75 mL). Filtration and washing as previously described gave the product (99 mg, 67% for two steps) as a yellow solid; δH (500 MHz, DMSO-d6) 2.54 (s, br, 4H, piperazine N(CH2)2), 3.06 (s, br, 4H, piperazine N(CH2)2), 3.60 (s, 2H, NCH2), 6.97 (s, br, 2H, NH2), 8.16 (s, 1H, bromopyridine H-6), 8.75 (s, 2H, pyrimidine H-4 & H-6), 9.10 (s, 1H, pyrimidine H-2);

1. customThis was prepared
2. filtrationFiltration
3. washwashing
4. customas previously described gave the product (99 mg, 67% for two steps) as a yellow solid

ORDレコード

ord-72b0943085e647009ad0105ee10e5e8e

出典データセット

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08088761B2