反应详情

温度

60 °C

To a stirred solution of [2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-thiophen-3-yl-ethyl]-carbamic acid tert-butyl ester (23 g, crude) in THF (100 mL) and methanol (100 mL) was added hydrazine hydrate (63 g, 1.26 mol). The mixture was heated to 60° C. for 2 hours and then cooled to 20° C. The reaction mixture was filtered and the filtration was concentrated to dryness. The residue was purified by column chromatography (methanol:dichloromethane, 1:50) to afford (2-amino-2-thiophen-3-yl-ethyl)-carbamic acid tert-butyl ester. (Yield 8.6 g, 57% for the two steps). LC-MS: [M+H]+ 243.

1. temperaturecooled to 20° C
2. filtrationThe reaction mixture was filtered
3. filtrationthe filtration
4. concentrationwas concentrated to dryness
5. customThe residue was purified by column chromatography (methanol:dichloromethane, 1:50)