HRID484839

反应详情

EQUATION

反应方程式

HRID 484839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 70 ml of ethyl alcohol was added 3.50 g of 1-(3-diethylaminopropyl)-3-phthalimido-4-chloroindazole. The mixture was added with 2.50 g of 85% hydrazine hydrate under cooling with ice and stirred for 3 hours under cooling with ice. The reaction mixture was filtered and the filtrate was condensed under reduced pressure. The condensed residue was added with 20 ml of water and extracted with chloroform. The chloroform layer was extracted with 2N-hydrochloric acid and the pH of the hydrochloric acid layer was adjusted to 10 with potassium carbonate. The alkali layer was extracted with chloroform. The chloroform layer was dried over anhydrous sodium sulfate and chloroform was removed under reduced pressure to give 2.03 g of 1-(3-diethylaminopropyl)-3-amino-4-chloroindazole having the following analytical values in a yield of 85%.

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. filtrationThe reaction mixture was filtered
  4. customcondensed under reduced pressure
  5. extractionextracted with chloroform
  6. extractionThe chloroform layer was extracted with 2N-hydrochloric acid
  7. extractionThe alkali layer was extracted with chloroform
  8. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate and chloroform
  9. customwas removed under reduced pressure