HRID606622

反应详情

EQUATION

反应方程式

HRID 606622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of isopropylhydrazine hydrochloride (0.53 g, 4.8 mmol), (3-oxo-propyl)-carbamic acid benzyl ester (1.0 g, 4.8 mmol), and Et3N (1.94 g, 192 mmol) in DMF (20 mL) was stirred at rt for 18 h. The solution was treated with 2-[3-(4-fluoro-phenyl)-2-nitro-allyl]-[1,3]dioxolane (1.02 g, 3.95 mmol) and stirred at 60° C. for 18 h. The mixture was cooled to rt and concentrated. The residue was partitioned between EtOAc and water. The organic layer was separated, dried (MgSO4), and concentrated. Purification by FCC gave the title compound.

WORKUP

后处理

  1. temperatureThe mixture was cooled to rt
  2. concentrationconcentrated
  3. customThe residue was partitioned between EtOAc and water
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customPurification by FCC