HRID1425568

反应详情

EQUATION

反应方程式

HRID 1425568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To tert-butyl 7-(benzyloxy)-9H-carbazol-2-ylcarbamate (200 mg, 0.51 mmol) was added 10 mL of a 4 M HCl in dioxane solution. The mixture was stirred at rt for 4 h and concentrated under reduced pressure. The residue was washed with ether (15 mL) and suspended in EtOAc (50 mL). To this suspension was added 10 mL of a NaHCO3 (sat.) and the mixture was stirred for 5 min. The organic layer was dried over MgSO4 and concentrated to afford 7-(benzyloxy)-9H-carbazol-2-amine as a brown solid (150 mg, 100%). 1H NMR (400 MHz, DMSO-d6) δ 11.33 (s, 1H), 7.99 (d, J=8.4 Hz, 1H), 7.92 (d, J=8.8 Hz, 1H), 7.42 (d, J=6.8 Hz, 2H), 7.34-7.21 (m, 3H), 7.27-7.23 (m, 1H), 7.00-6.97 (m, 2H), 6.81 (dd, J=8.8, 2.4 Hz, 1H), 5.12 (s, 2H); MS (ESI) m/z 289 (M+H+).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. washThe residue was washed with ether (15 mL)
  3. additionTo this suspension was added 10 mL of a NaHCO3 (sat.)
  4. stirringthe mixture was stirred for 5 min
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated