Citric Acid → 2-(4-methyl-1-piperidyl)-N-[[2-(trifluoromethyl)-1H-indol-5-yl]methyl]-pyrimidine-5-carboxamide

To a stirred solution of HATU (34.4 mg, 0.090 mmol) in 1 ml DMF was added (2-(4-methyl-1-piperidinyl)-5-pyrimidinecarboxylic acid) (Matrix Scientific, 20 mg, 0.090 mmol) in 0.5 ml DMF, followed by DIPEA (0.016 ml, 0.090 mmol) and finally {[2-(trifluoromethyl)-1H-indol-5-yl]methyl}amine (Intermediate 4, 22.66 mg, 0.090 mmol) in 1 ml DMF. Stirring was continued for 16 hours. 1M citric acid solution (10 ml) was added and the mixture was then extracted with ethyl acetate (20 ml). The organic extract was then washed with 1M citric acid solution (10 ml), brine (10 ml), dried (MgSO4), filtered and evaporated to dryness. The resulting residues where then purified on the MDAP to dryness to give the title compound (19 mg);

1. extractionthe mixture was then extracted with ethyl acetate (20 ml)
2. extractionThe organic extract
3. washwas then washed with 1M citric acid solution (10 ml), brine (10 ml)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated to dryness
7. customThe resulting residues where then purified on the MDAP to dryness

ORDレコード

ord-b3a424193d0047daabfbaef6aad04fa9

出典データセット

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08377941B2