HRID1619980

反应详情

EQUATION

反应方程式

HRID 1619980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

403 mg (2.74 mmol) 4-cyano-benzoic acid and 967 mg (3.01 mmol) TBTU are added to 40 ml DMF and the mixture is stirred for 30 min at RT, then 791 μl (5.47 mmol) diisopropylamine and 600 mg (2.74 mmol) 6-(4-amino-3-hydroxy-phenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one are added and the mixture is stirred overnight. The reaction mixture is mixed with water and extracted with DCM. The org. phase is again washed with water, dried on sodium sulphate and concentrated by rotary evaporation i. V. The residue is extracted with methanol, filtered off, washed with methanol and then dried in the vacuum dryer at 50° C.

WORKUP

后处理

  1. stirringthe mixture is stirred overnight
  2. extractionextracted with DCM
  3. washphase is again washed with water
  4. customdried on sodium sulphate
  5. concentrationconcentrated by rotary evaporation i
  6. extractionThe residue is extracted with methanol
  7. filtrationfiltered off
  8. washwashed with methanol
  9. customdried in the vacuum dryer at 50° C.