HRID1378437

反应详情

EQUATION

反应方程式

HRID 1378437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of the product from Step 1 (3.23 g, 0.0115 mol), 1-phenylcyclobutylamine (1.73 g, 0.0126 mol) (A. Kalir and Z. Pelah, Israel J. Chem. 5:223 (1967)), N-methylmorpholine (2.74 ml, 0.0249 mol) and dioxane (40 ml) was refluxed, under nitrogen for 18 hours and concentrated in vacuo. The residue was mixed with EtOAc and concentrated to give a solid which was recrystallized from EtOAc-hexane to give 1.7 g, mp 204°-205° C. of the titled product.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. additionThe residue was mixed with EtOAc
  3. concentrationconcentrated
  4. customto give a solid which
  5. customwas recrystallized from EtOAc-hexane