Methylhydrazine → HCID 67548813、化合物

HRID 2261010ノート

反応式

HRID 2261010 の反応式
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

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. extractionthe aq. layer was extracted with ethyl acetate
  3. customthe combined organic layers were dried
  4. concentrationconcentrated in vacuo
  5. 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

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