Iodoethane → (3-amino-1-ethyl-1H-pyrazol-4-yl)-phenyl-methanone

HRID 494369노트

반응식

HRID 494369 반응식
[NH2:1][C:2]1[C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:8])=[CH:5][NH:4][N:3]=1.[H-].[Na+].[CH2:17](I)[CH3:18]>CN(C=O)C.C(OCC)(=O)C>[NH2:1][C:2]1[C:6]([C:7]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)=[O:8])=[CH:5][N:4]([CH2:17][CH3:18])[N:3]=1

참가 물질

6

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 178509267HCID 178509267, 화합물

생성물 1

HCID 68866724(3-amino-1-ethyl-1H-pyrazol-4-yl)-phenyl-methanone

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a vigorously stirring solution of (3-amino-1H-pyrazol-4-yl)-phenyl-methanone (0.1 g, 0.53 mmol) in dry DMF at RT is added sodium hydride (0.023 g, 0.57 mmol). After 1 h, ethyl iodide (0.042 mL, 0.53 mmol) is added and stirring is continued for 4 h. The reaction mixture is diluted with ethyl acetate, washed with water, brine and dried over anhydrous sodium sulfate. The organic filtrate is concentrated and the crude is chromatographed on silica gel using 50% ethyl acetate in hexanes to provide (3-amino-1-ethyl-1H-pyrazol-4-yl)-phenyl-methanone.

후처리

  1. waitis continued for 4 h
  2. washwashed with water, brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationThe organic filtrate is concentrated
  5. customthe crude is chromatographed on silica gel using 50% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-8126096e5b3b44298db9109978e0fb0d
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538135B2

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