HRID1915922

反应详情

EQUATION

反应方程式

HRID 1915922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a microwave reaction vial was added 5-chloro-1-methyl-4-nitro-1H-pyrazole (500 mg, 3.10 mmol), tert-butyl 1,4-diazepane-1-carboxylate (744 mg, 3.72 mmol). Ethanol (15 mL) and diisopropylethylamine (3.23 mL, 18.57 mmol) were added and the mixture was irradiated with a microwave for 60 min at 130° C. The mixture was cooled, concentrated and purified via flash chromatography, ethyl acetate/heptane 0% to 100% to afford yellow oil tert-butyl 4-(2-methyl-4-nitro-pyrazol-3-yl)-1,4-diazepane-1-carboxylate (690 mg, 69%).

WORKUP

后处理

  1. customTo a microwave reaction
  2. customthe mixture was irradiated with a microwave for 60 min at 130° C
  3. temperatureThe mixture was cooled
  4. concentrationconcentrated
  5. custompurified via flash chromatography, ethyl acetate/heptane 0% to 100%