HRID349286

反应详情

EQUATION

反应方程式

HRID 349286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of [1-(3,5-Bis-trifluoromethyl-benzyl)-5-phenyl-1H-[1,2,3]triazol-4-yl]-(3-phenyl-5-trimethylsilanyl-3H-[1,2,3]triazol-4-yl)-methanone (0.050 g, 0.08 mmol) in THF (2 mL) add t-butyl ammonium flouride (1 M soln. in THF, 1.2 mL, 1.2 mmol) and acetic acid (120 μL, 2.0 mmol) and heat at 65° C. After 72 h., remove from heat, and quench with sat. aq. NH4C1 and H2O. Extract with EtOAc, dry over MgSO4, filter, and purify by flash chromatography (EtOAc/Hexane 0%–50%) to give the title compound. 1H NMR (300 MHz, CDCl3) δ 8.88 (s, 1H), 7.75 (s, 1H), 7.57–7.29 (m, 10H), 7.09 (m, 2H), 5.50 (s, 2H).

WORKUP

后处理

  1. customremove
  2. temperaturefrom heat
  3. customquench with sat. aq. NH4C1 and H2O
  4. extractionExtract with EtOAc
  5. dry with materialdry over MgSO4
  6. filtrationfilter
  7. custompurify by flash chromatography (EtOAc/Hexane 0%–50%)