HCID 44596871、化合物 → HCID 13876050、化合物
反応式
[CH3:1][O:2][C:3]1[CH:30]=[CH:29][C:6]([CH2:7][C@:8]2([CH3:28])[C:12](=[O:13])[O:11][C@@H](C3C=CC=CC=3)[N:9]2C(C2C=CC=CC=2)=O)=[CH:5][CH:4]=1>Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][C@:8]([CH3:28])([C:12]([OH:13])=[O:11])[NH2:9])=[CH:29][CH:30]=1参加物
3
実験手順
Compound 2.3 (2.2 g, 0.0055 mol) were suspended in 20 mL of concentrated HCl solution. After nitrogen flush, the mixture was heated under reflux for 3 hours. After filtration and removal of the HCl solution, the white precipitate was dried. 1H NMR δ 7.24 (d, 2H, J=6 Hz), 6.91 (d, 2H, J=6 Hz), 3.77 (3H, s), 3.26 (d, 1H, J=14 Hz), 3.13 (d, 1H, J=14 Hz), 1.66 (s, 3H); C NMR 173.8, 161.3, 132.9, 115.9, 62.4, 56.4, 43.5, 23.2; ESI MS 210 (M+1). The product was used in the next step without purification.
後処理
- customAfter nitrogen flush
- temperaturethe mixture was heated
- temperatureunder reflux for 3 hours
- filtrationAfter filtration and removal of the HCl solution
- customthe white precipitate was dried
- customThe product was used in the next step without purification
出典と根拠
- ORDレコード
- ord-6d7e6fc4cc314556bf2c78b86844bfff
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08048895B2
反応ノート
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