HRID241448

反应详情

EQUATION

反应方程式

HRID 241448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 1-[6-(trifluoromethyl)-3-pyridyl]propan-1-ol (2.010 g, 9.796 mmol) in DCM (40 mL). Add 3,3,3-Triacetoxy-3-iodophthalide (4.712 g, 10.776 mmol), and stir for 16 hours. Dilute with DCM (100 mL). Wash with 0.5 N NaOH (100 mL). Dry the organic extracts over Na2SO4; filter; collect the filtrate; and concentrate the filtrate under reduced pressure to give the title compound (1.910 g, 96% yield) as a white solid. 1H NMR (400.43 MHz, d6-DMSO) δ 9.21 (dd, J=0.5, 1.4 Hz, 1H), 8.51-8.49 (m, 1H), 8.03 (dd, J=0.7, 8.1 Hz, 1H), 3.12 (q, J=7.1 Hz, 2H), 1.05 (t, J=7.1 Hz, 3H).

WORKUP

后处理

  1. washWash with 0.5 N NaOH (100 mL)
  2. dry with materialDry the organic extracts over Na2SO4
  3. filtrationfilter
  4. customcollect the filtrate
  5. concentrationand concentrate the filtrate under reduced pressure