HRID929510

反应详情

EQUATION

反应方程式

HRID 929510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Intermediate 42 (100 mg, 0.33 mmol) was dissolved in dry THF (1 mL), ethyl trifluoroacetate (30 μl 0.39 mmol) was added and the reaction was refluxed for 18 hours. The reaction was cooled to RT, evaporated and the residue chromatographed from EtOAc to give compound 53 (49 mg, 37%) as a white solid: Mp 150-154° C. 1H NMR (500 MHz, DMSO-d6) δ 8.59 (s, 1H), 7.47 (d, J=9.0 Hz, 2H), 7.22 (d, J=8.6 Hz, 2H), 6.27 (d, J=7.6 Hz, 1H), 4.15 (d, J=13.1 Hz, 1H), 3.80 (d, J=11.1 Hz, 2H), 3.38 (t, J=11.9 Hz, 1H), 3.11 (t, J=12.1 Hz, 1H), 1.94 (t, J=15.2 Hz, 2H), 1.46-1.34 (m, 2H). Purity 100%. HRMS calculated for C15H15F6N3O3+H+ 400.1096. found (ESI(+), [M+H]) 400.1078.

WORKUP

后处理

  1. temperaturethe reaction was refluxed for 18 hours
  2. customevaporated
  3. customthe residue chromatographed from EtOAc