HRID708491

反应详情

EQUATION

反应方程式

HRID 708491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of tert-butyl (3-((imino(methylthio)methyl)amino)propyl)carbamate (32.1 mg, 87 μmol) in dioxane (1 mL, ratio: 2) at rt was added triethylamine (30 μL, 0.22 mmol), 1-(((Z)-(2-(((2R,3S)-2-((4-(aminomethyl)-2H-1,2,3-triazol-2-yl)methyl)-4-oxo-1-sulfoazetidin-3-yl)amino)-1-(2-aminothiazol-4-yl)-2-oxoethylidene)amino)oxy)cyclopropanecarboxylic acid (example 19, 23 mg, 43 μmol), and DMF (0.5 mL, ratio: 1). After heated to 60° C. for 17 h, the reaction mixture was diluted with EtOAc and water. The aqueous layer was separated, concentrated in vacuo, azeotroped with toluene, and dried on high vac to give the title compound (assumed quantitative). LCMS: Rt=0.51 min, m/z=729.6 (M+1), Method 2m_acidic.

WORKUP

后处理

  1. customThe aqueous layer was separated
  2. concentrationconcentrated in vacuo
  3. customazeotroped with toluene
  4. customdried on high vac