3-Iodoaniline → N-(3-iodophenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide

HRID 1099681

반응식

HRID 1099681 반응식
[I:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].[CH3:9][N:10]1[C:14]([C:15](Cl)=[O:16])=[CH:13][C:12]([CH3:18])=[N:11]1>N1C=CC=CC=1.ClCCCl>[I:1][C:2]1[CH:3]=[C:4]([NH:5][C:15]([C:14]2[N:10]([CH3:9])[N:11]=[C:12]([CH3:18])[CH:13]=2)=[O:16])[CH:6]=[CH:7][CH:8]=1

참가 물질

5

반응물 2

HCID 122713-IodoanilineHCID 27362992,5-Dimethyl-2H-pyrazole-3-carbonyl chloride

생성물 1

HCID 57657852N-(3-iodophenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 1049Pyridine용매

실험 절차

To a solution of 3-iodoaniline (131 mg, 0.60 mmol) in 1.5 ml pyridine at room temperature was added over 2 minutes a solution of 1,3-dimethylpyrazole-5-carbonyl chloride (79 mg, 0.50 mmol) in 0.3 ml 1,2-dichloroethane. The reaction was stirred at room temperature for 30 minutes, quenched into a NaHCO3 solution, and extracted into EtOAc. The EtOAc solution was washed with NaHCO3 solution, brine, dried with anhydrous Na2SO4 and rotary evaporated. The resultant gummy solid was recrystallized from hexane/EtOAc to give the title compound as solid white needles (135 mg, 80%).

후처리

  1. customquenched into a NaHCO3 solution
  2. extractionextracted into EtOAc
  3. washThe EtOAc solution was washed with NaHCO3 solution, brine
  4. dry with materialdried with anhydrous Na2SO4 and rotary evaporated
  5. customThe resultant gummy solid was recrystallized from hexane/EtOAc

출처 및 근거

ORD 기록
ord-d3f52e943fbc4d4e9dbc829739279d92
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143410B2

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