Methylhydrazine → HCID 67548813、化合物
反応式
F[C:2]1[C:7]([CH:8]=O)=[C:6]([I:10])[CH:5]=[CH:4][N:3]=1.[CH3:11][NH:12][NH2:13]>>[I:10][C:6]1[CH:5]=[CH:4][N:3]=[C:2]2[N:12]([CH3:11])[N:13]=[CH:8][C:7]=12参加物
3
実験手順
227 mg of 2-fluoro-4-iodo-pyridine-3-carbaldehyde (0.9 mmol, 1 eq.; prepared as described in J. Org. Chem. 1993, 58, 7832) were dissolved in 3.6 mL 1-PrOH, treated with 72 μL methyl hydrazine (1.36 mmol, 1.5 eq.) and heated to 100° C. for 30 min (Biotage Initiator 60®). The reaction mixture was concentrated in vacuo, the residue was partioned between water and ethyl acetate, the aq. layer was extracted with ethyl acetate, the combined organic layers were dried and concentrated in vacuo to provide the crude target compound.
後処理
- concentrationThe reaction mixture was concentrated in vacuo
- extractionthe aq. layer was extracted with ethyl acetate
- customthe combined organic layers were dried
- concentrationconcentrated in vacuo
- customto provide the crude target compound
出典と根拠
- ORDレコード
- ord-48cca360379648a7a0de081b6ed67cb3
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07846928B2
反応ノート
読み込み中…