HRID1038129

反应详情

EQUATION

反应方程式

HRID 1038129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Suspension of 5-nitro-1H-indazole-3-carboxylic acid methyl ester 18AP (7 g, 31.67 mmol) in THF (130 ml) and DCM (15 ml) was added to a NaH (60% in Mineral Oil, 1.61 g, 41.17 mmol) at 0° C. H2 gas was evolved. Chlorotriphenyl methane (8.83 g, 31.67 mmol) was added after stirring for 20 min at 0° C. Reaction mixture was subjected to heat at 60° C. for overnight. It was then cooled to room temperature and concentrated under reduced pressure. Solid was redissolved in DCM and filtered. Filtrate was concentrated under reduced pressure to give desired 5-nitro-1-trityl-1H-indazole-3-carboxylic acid methyl ester 19AP (12.95 g, 88%).

WORKUP

后处理

  1. customReaction mixture
  2. temperatureto heat at 60° C. for overnight
  3. temperatureIt was then cooled to room temperature
  4. concentrationconcentrated under reduced pressure
  5. dissolutionSolid was redissolved in DCM
  6. filtrationfiltered
  7. concentrationFiltrate was concentrated under reduced pressure