Triethyl orthoacetate → HCID 19349977、化合物
反応式
[I:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([NH:7][NH2:8])=[O:6].[CH2:12](OC(OCC)(OCC)C)[CH3:13]>C(O)(=O)C>[I:1][C:2]1[CH:3]=[C:4]([C:5]2[O:6][C:12]([CH3:13])=[N:8][N:7]=2)[CH:9]=[CH:10][CH:11]=1参加物
4
反応条件
- 温度
- 150 °C
実験手順
In a schlenck tube, a mixture of 3-iodobenzohydrazide (510 mg, 1.95 mmol) and 1,1,1-triethoxyethane (1.14 ml, 6.23 mmol) in acetic acid (15 ml) was heated at 150° C. for 3 h. The solvent was evaporated and the crude redissolved in ethyl acetate and washed with 4% solution of NaHCO3, water and brine. The organic layer was dried, filtered and concentrated under vacuum to give the title compound as a white solid (92% yield).
後処理
- customThe solvent was evaporated
- dissolutionthe crude redissolved in ethyl acetate
- washwashed with 4% solution of NaHCO3, water and brine
- customThe organic layer was dried
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-b834c3bf6f8e474790aa81fa7c23d952
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536165B2
反応ノート
読み込み中…