HRID40687

反应详情

EQUATION

反应方程式

HRID 40687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,2-Diethoxy-N-(2-fluorobenzyl)acetamide (4.1 g, 16.0 mmol) was stirred in concentrated sulfuric acid (10 mL) for 16 hours. The reaction mixture was poured onto ice and neutralized by the addition of ammonium hydroxide forming a precipitate which was removed by filtration. The filtrate was extracted with ethyl acetate three times, and the combined organic phases were rinsed with brine then dried (Na2SO4) and concentrated to dryness affording an oily solid. Trituration with ether afforded the title compound (1.56 g, 9.6 mmol, 60% over 2 steps). LC-MS (3) Rt=1.00 min; m/z (ESI+) 164 (M+H).

WORKUP

后处理

  1. additionThe reaction mixture was poured onto ice
  2. customwas removed by filtration
  3. extractionThe filtrate was extracted with ethyl acetate three times
  4. washthe combined organic phases were rinsed with brine
  5. dry with materialthen dried (Na2SO4)
  6. concentrationconcentrated to dryness
  7. customaffording an oily solid