HRID1663174

反应详情

EQUATION

反应方程式

HRID 1663174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1-(2-amino-pyridin-4-ylmethyl)-1H-benzo[d][1,3]oxazine-2,4-dione (600 mg, see preparation 7b) in pyridine (5 ml) was added acetoxyacetyl chloride (0.29 ml). The reaction mixture was stirred at room temperature for 30 minutes. The solvent was evaporated under reduced pressure. The remaining oil was dissolved in EtOAc and washed with water and brine. The organic layer was concentrated to ca. 10 ml under reduced pressure. The resulting solid material was isolated by filtration and dried in vacuo, affording acetic acid [4-(2,4-dioxo-4H-benzo[d][1,3]oxazin-1-ylmethyl)-pyridin-2-ylcarbamoyl]-methyl ester.

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionThe remaining oil was dissolved in EtOAc
  3. washwashed with water and brine
  4. concentrationThe organic layer was concentrated to ca. 10 ml under reduced pressure
  5. customThe resulting solid material was isolated by filtration
  6. customdried in vacuo