Ammonium formate → HCID 58484354, 화합물

HRID 42705노트

반응식

HRID 42705 반응식
Cl[C:2]1[C:3](=[O:16])[N:4]([CH3:15])[N:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]1.C([O-])=O.[NH4+].ClCCl.CO>[Pd].CO>[CH3:15][N:4]1[C:3](=[O:16])[CH:2]=[C:7]([N:8]2[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]2)[CH:6]=[N:5]1

참가 물질

6

반응물 3

HCID 2723923Ammonium formate2회HCID 170880204-Chloro-2-methyl-5-(4-methylpiperazin-1-yl)pyridazin-3(2H)-oneHCID 21226129Dichloromethane methanol

생성물 1

HCID 58484354HCID 58484354, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a mixture of 4-chloro-2-methyl-5-(4-methylpiperazin-1-yl)pyridazin-3(2H)-one (4.85 g, 20 mmol) and 10% Pd/C catalyst (1.14 g) in methanol (100 ml) was added ammonium formate (2.90 g, 46 mmol), and the mixture was refluxed under argon with TLC monitoring (dichloromethane:methanol (9:1)). Further portions of ammonium formate were added until the starting material was completely consumed. The catalyst was filtered off and washed with methanol, then the solvent was evaporated under reduced pressure. The residue was taken up in water (30 ml) and extracted with dichloromethane (4×40 ml). The combined extracts were washed with water, dried (Na2SO4) and evaporated. The crude product was purified by recrystallization from ethyl acetate:light petroleum.

후처리

  1. customwas completely consumed
  2. filtrationThe catalyst was filtered off
  3. washwashed with methanol
  4. customthe solvent was evaporated under reduced pressure
  5. extractionextracted with dichloromethane (4×40 ml)
  6. washThe combined extracts were washed with water
  7. dry with materialdried (Na2SO4)
  8. customevaporated
  9. customThe crude product was purified by recrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-481462f735094066b3bc31c610911691
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536210B2

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