HRID606621

反应详情

EQUATION

反应方程式

HRID 606621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of isopropylhydrazine hydrochloride (1.07 g, 9.7 mmol) and (3-oxo-propyl)-carbamic acid benzyl ester (2.0 g, 9.7 mmol) in Et3N (20 mL) was heated at 60° C. After 1 h, 2-[3-(4-fluoro-phenyl)-2-nitro-allyl]-[1,3]dioxolane (2.2 g, 8.7 mmol) was added. After 16 h at 60° C., 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. waitAfter 16 h at 60° C.
  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