반응식
[CH3:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][N:7]2[CH:11]=[CH:10][C:9]([N+:12]([O-])=O)=[N:8]2)=[CH:4][CH:3]=1>O1CCCC1.NN.[Ni]>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]2[CH:11]=[CH:10][C:9]([NH2:12])=[N:8]2)=[CH:15][CH:16]=1참가 물질
5
실험 절차
To a solution containing 1-(4-methyl-benzyl)-3-nitro-1H-pyrazole (92 mg, 0.42 mmol) in tetrahydrofuran (2 mL), anhydrous hydrazine (100 μL) was added to the clear solution. Raney nickel (˜100 mg washed 3 times with 5 mL of anhydrous tetrahydrofuran) was then added in tetrahydrofuran (300 μL). Gas evolved from the mixture and the reaction was allowed to proceed for 5 min, after which time the raney nickel was removed by filtration through a celite plug. The solvent was removed in vacuo to afford 1-(4-methyl-benzyl)-1H-pyrazol-3-ylamine as a yellow oil which was used in the following step with no further purification.
후처리
- additionwas added to the clear solution
- customafter which time the raney nickel was removed by filtration through a celite plug
- customThe solvent was removed in vacuo
출처 및 근거
- ORD 기록
- ord-f11207cfe36b4a66a84f0f32ba581c7f
- 출처 데이터셋
- uspto-grants-2011_05
- 특허 번호
- US07935699B2
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