HRID1760029

反应详情

EQUATION

反应方程式

HRID 1760029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2-chloro-5-(Boc-amino)phenyl)acetic acid (2.8 g; 9.8 mmol; from step (iv) above) in acetone (100 mL) was added K2CO3 (2.1 g, 15 mmol). EtI (70.6 g; 150 mmol) was then added whilst the reaction mixture was stirred and refluxed. The solution was concentrated, and the resultant mixture was partitioned between ether and water (1:1; 60 mL). The organic layer was separated, and the water layer was extracted once with ether (30 mL). The combined organic phase was washed with water, dried (Na2SO4), and concentrated to yield 3.0 g (98%) of the sub-title compound.

WORKUP

后处理

  1. temperaturerefluxed
  2. concentrationThe solution was concentrated
  3. customthe resultant mixture was partitioned between ether and water (1:1; 60 mL)
  4. customThe organic layer was separated
  5. extractionthe water layer was extracted once with ether (30 mL)
  6. washThe combined organic phase was washed with water
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated