HRID351839

反应详情

EQUATION

反应方程式

HRID 351839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-(2,4-Dimethoxy-benzyl)-8-isopropyl-6-oxo-5,6-dihydro-4H-2,5,10b-triaza-benzo[e]azulene-3-carboxylic acid ethyl ester (410 mg, 0.9 mmol) was suspended in CH2Cl2 (3.0 mL), cooled in ice, and diluted slowly with trifluoroacetic acid (2.0 mL). The resulting solution was treated at 5° C. with trifluoromethanesulfonic acid (1.0 mL, 1.3 mmol). The red solution was stirred at room temperature for 2 h. The mixture was then evaporated and dissolved in CH2Cl2 (20 mL), washed with sodium hydrogen carbonate (10%, 2×5 mL) and the organic layer was dried (Na2SO4) and evaporated. Trituration with EtOAc. Yield: 250 mg (90%). m/z 313 (MH).

WORKUP

后处理

  1. temperaturecooled in ice
  2. customThe mixture was then evaporated
  3. dissolutiondissolved in CH2Cl2 (20 mL)
  4. washwashed with sodium hydrogen carbonate (10%, 2×5 mL)
  5. dry with materialthe organic layer was dried (Na2SO4)
  6. customevaporated