反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([NH:9][NH2:10])=[O:8])=[CH:5][CH:4]=1.[C:13](Cl)(=[O:15])[CH3:14]>C1COCC1>[C:13]([NH:10][NH:9][C:7](=[O:8])[C:6]1[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=1)(=[O:15])[CH3:14]参加物
4
実験手順
To 40 mL of THF were added 1.8 g (10.8 mmol) of 4-methoxybenzoylhydrazine, 0.9 g (11.5 mmol) of acetyl chloride and 1.1 g of TEA. The reaction mixture was stirred for 1 hour, followed by evaporation off ca. ½ volume of THF. The product was precipitated into methanol, filtered and dried over night under vacuum. Yield was 2.14 g (95%). MS (EI, m/e) calcd for C10H12N2O3 208, found 208 M+, 6.7); mp 146-148° C.
後処理
- customfollowed by evaporation off ca. ½ volume of THF
- customThe product was precipitated into methanol
- filtrationfiltered
- customdried over night under vacuum
出典と根拠
- ORDレコード
- ord-5372c1b158d64bbb9963923c5df5e946
- 出典データセット
- uspto-grants-2004_11
- 特許番号
- US06815528B2
関連ノート
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