HRID571044

反应详情

EQUATION

反应方程式

HRID 571044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To tert-butyl[5-(benzyloxy)-1-(biphenyl-3-yl)-4-oxo-1,4-dihydropyridin-2-yl]carbamate (4.68 g, 10 mmol) was added TFA-DCM (1:1, 60 mL), and the resulting solution was stirred for 1 h at rt. The solution was then concentrated and treated with saturated aq. NaHCO3-EtOAc. The organic layer was separated, washed with brine, dried (Na2SO4), filtered, and concentrated to give 2-amino-5-(benzyloxy)-1-(biphenyl-3-yl)pyridin-4(1H)-one as a slightly yellow solid 1H NMR (500 MHz, DMSO): ä 7.82 (ddd, J=7.8, 1.8, 1.0 Hz, 1 H); 7.76-7.73 (m, 2 H); 7.67-7.61 (m, 2 H); 7.53-7.47 (m, 2 H); 7.43-7.34 (m, 6 H); 7.33-7.29 (m, 1 H); 7.04 (s, 1 H); 5.65 (s, 2 H); 5.49 (s, 1 H); 4.89 (s, 2 H).

WORKUP

后处理

  1. concentrationThe solution was then concentrated
  2. additiontreated with saturated aq. NaHCO3-EtOAc
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated