HRID38817

反应详情

EQUATION

反应方程式

HRID 38817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

N-{2-Chloro-5-[1-[(4-methylphenyl)sulfonyl]-4-(1H-tetrazol-5-yl)-1H-indazol-6-yl]-3-pyridinyl}methanesulfonamide (1.3 g, 2.385 mmol) and chloro acetylchloride (0.285 ml, 3.58 mmol) were placed in toluene (35 ml) and the mixture heated at 105° C. for 30 mins. The temperature was increased to 115° C. and the mixture heated for 1 h. The mixture was cooled to room temperature and the solvent removed in vacuo. This was purified by chromatography on a silica (100 g) cartridge eluting with 0-100% ethyl acetate in cyclohexane followed by 0-20% methanol in dichloromethane, to give the title compound as a yellow solid (0.332 g).

WORKUP

后处理

  1. temperatureThe temperature was increased to 115° C.
  2. temperaturethe mixture heated for 1 h
  3. temperatureThe mixture was cooled to room temperature
  4. customthe solvent removed in vacuo
  5. customThis was purified by chromatography on a silica (100 g) cartridge
  6. washeluting with 0-100% ethyl acetate in cyclohexane