Hydrochloric Acid → HCID 178502451、化合物

To a solution of (2S)-2-(methoxycarbonylamino)-3-methyl-butanoic acid (644.5 mg, 3.68 mmol) in DMF (25 mL) at 0° C. is added HATU (1.4 g, 3.68 mmol), DIPEA (2.5 mL, 14.57 mmol) followed by 4-iodo-2-[(2S,4S)-4-methylpyrrolidin-2-yl]-1H-imidazole as HCl salt (1.28 g, 3.64 mmol). The reaction mixture is stirred at rt for 20 hours, diluted with EtOAc and H2O. The organic phase is separated, washed with H2O, dried over Na2SO4, filtered and concentrated to dryness. The residue is purified by flash column chromatography on silica gel (0 to 100% EtOAC/Hexane) to afford methyl N-[(1S)-1-[(2S,4S)-2-(4-iodo-1H-imidazol-2-yl)-4-methyl-pyrrolidine-1-carbonyl]-2-methyl-propyl]carbamate (1.3 g, 87.3%) as a white solid.

1. customThe organic phase is separated
2. washwashed with H2O
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. customThe residue is purified by flash column chromatography on silica gel (0 to 100% EtOAC/Hexane)

ORDレコード

ord-1ae00e50f43f4ba2b0b69ae7ec013d39

出典データセット

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08779156B2