HRID1262408

反应详情

EQUATION

反应方程式

HRID 1262408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-(2-Methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazine-2-carbonitrile (151 mg, 0.603 mmol) and 9.5 M of Sodium hydroxide in Water (0.20 mL, 1.9 mmol) were combined in Ethanol (6.0 mL) in a vial, which was then heated to reflux for 90 min. The mixture was removed from the heat and treated with 3.00 M of Hydrogen Chloride in Water (1.00 mL, 3.0 mmol), generating a precipitate, which was diluted with water (2 mL), stirred vigorously (thick suspension) then collected by filtration, washing with water (2×8 mL) and drying on the Buchner then in vacuo to afford 7-(2-Methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazine-2-carboxylic acid (145 mg, 89%). LCMS (HPLC): 0.76 min, m/z=270 (M+H); 1H-NMR (DMSO-d6): 13.55 (br s, 1H), 9.27 (s, 1H), 7.73 (d, 1H, J=7.5 Hz), 7.49 (m, 1H), 7.39 (d, 1H, J=4.6 Hz), 7.25 (s, 1H), 7.23 (d, 1H, J=4.6 Hz), 7.12 (m, 1H), 3.81 (s, 3H).

WORKUP

后处理

  1. temperaturewas then heated
  2. temperatureto reflux for 90 min
  3. customThe mixture was removed from the
  4. temperatureheat
  5. filtrationthen collected by filtration
  6. washwashing with water (2×8 mL)
  7. customdrying on the Buchner