Diisopropylethylamine → 1-(4-[1,3]Dioxolan-2-yl-piperidin-1-yl)-3-[2-methyl-4-(3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-phenyl]-propan-1-one

HBTU (327 mg, 0.86 mmol) was added to a solution of 4-[1,3]dioxolan-2-yl-piperidine from Example E33 (143 mg, 0.91 mmol) and 3-[2-methyl-4-(3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-phenyl]-propionic acid from Example E45 (320 mg, 0.82 mmol) in dichloromethane (20 ml) and DIEA (0.7 ml, 4.02 mmol) and the mixture was stirred for 20 h at room temperature. Dichloromethane was added and the solution was washed with saturated NaHCO3 then brine, dried and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 4% methanol:96% dichloro-methane to 8% methanol:92% dichloromethane) to give a white solid identified as the title compound (359 mg, 83%).

1. washthe solution was washed with saturated NaHCO3
2. dry with materialbrine, dried
3. concentrationconcentrated in vacuo
4. customThe residue was purified by flash chromatography on silica gel (eluant; 4% methanol:96% dichloro-methane to 8% methanol:92% dichloromethane)
5. customto give a white solid

ORDレコード

ord-6b92ee27981445be8f327309078db5d3

出典データセット

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08202858B2