反应详情

A solution of [2-(1,3-dioxo-1,3-dihydro-isoindol-2-yloxy)-ethyl]-methyl-carbamic acid tert-butyl ester (4.50 g, 14.0 mmol) in dichloromethane (40 mL) was treated with methylhydrazine (0.78 mL, 14.7 mmol) and the reaction mixture was stirred 6 h at ambient temperature. Diethyl ether (80 mL) was added and the heterogeneous solution was allowed to stand overnight. The precipitate was removed by filtration and was washed with ether (80 mL). The filtrate was further concentrated and the resultant precipitate was filtered and the second filtrate concentrated to afford (2-Aminooxy-ethyl)-methyl-carbamic acid tert-butyl ester (2.83 g) as a viscous oil: 1H NMR (400 MHz, CDCl3) δ 3.73 (t, J=5.2 Hz, 2H), 5.45 (br s, NH2), 3.46 and 3.42 (br s, 2H), 2.86 br s, 3H), 1.25 (br s, 9H); MS (APCI+)=191.1.

1. waitto stand overnight
2. customThe precipitate was removed by filtration
3. washwas washed with ether (80 mL)
4. concentrationThe filtrate was further concentrated
5. filtrationthe resultant precipitate was filtered
6. concentrationthe second filtrate concentrated