HRID1917267

反应详情

EQUATION

反应方程式

HRID 1917267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the product from Step A (2.0 g, 5.3 g) in MeOH (30 mL) was added p-TsOH.H2O. After 18 h, the reaction was diluted with satd. aq. NaHCO3 and extracted with EtOAc (2×). The combined organic layers were dried and concentrated to give the 1.53 g (99%) of the title compound. MS (ESI): exact mass calcd. for C19H18N2O, 290.14; m/z found, 291.4 [M+H]+. 1H NMR (CDCl3): 8.00-7.98 (m, 2H), 7.45-7.43 (m, 3H), 7.32-7.28 (m, 4H), 7.23-7.20 (m, 1H), 4.74 (d, J=4.8, 2H), 4.33 (s, 2H), 3.62 (t, J=5.1, 1H), 2.42 (s, 3H).

WORKUP

后处理

  1. additionthe reaction was diluted with satd
  2. extractionaq. NaHCO3 and extracted with EtOAc (2×)
  3. customThe combined organic layers were dried
  4. concentrationconcentrated