HRID2402795

反应详情

EQUATION

反应方程式

HRID 2402795 的结构方程式

PROCEDURE

实验过程

A quantity of 16 ml (295.41 mmol) of nitromethane was admixed with 436 μl (2.50 mmol) of N,N-diisopropylethylamine and the yellow solution was stirred at RT for 1 h. Then 2.0 g (8.34 mmol) of the compound from Example 111A were added and the mixture was stirred overnight at RT. All of the volatile constituents were removed on a rotary evaporator. The residue was dissolved in 9 ml of isopropanol in the heat of boiling, and the solution was then cooled to 0° C. The white solid precipitated was filtered off with suction and washed with a little cold isopropanol. Drying in an HV gave 1.18 g (47% of theory) of the title compound.

WORKUP

后处理

  1. stirringthe mixture was stirred overnight at RT
  2. customAll of the volatile constituents were removed on a rotary evaporator
  3. dissolutionThe residue was dissolved in 9 ml of isopropanol in the
  4. temperatureheat
  5. temperaturethe solution was then cooled to 0° C
  6. customThe white solid precipitated
  7. filtrationwas filtered off with suction
  8. washwashed with a little cold isopropanol
  9. customDrying in an HV