Ethanol → HCID 15134190、化合物
反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:8]([C:12]([OH:14])=[O:13])=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1.OS(O)(=O)=O.[CH3:20][CH2:21]O>C(Cl)Cl>[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:8]([C:12]([O:14][CH2:20][CH3:21])=[O:13])=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1参加物
5
実験手順
To a slurry of compound 73a (3.1 g, 16 mmol) in EtOH (50 mL) was added concentrated H2SO4 (1.0 mL) and the resultant slurry was refluxed overnight. The homogeneous solution was cooled, diluted with DCM (300 mL), washed with 1N NaOH (1×100 mL), dried (Na2SO4), and concentrated in vacuo to give compound 73b as an off-white solid. Mass spectrum (LCMS, ESI pos.) Calcd. For C13H13NO2: 216.2 (M+H). found 216.2.
後処理
- temperaturethe resultant slurry was refluxed overnight
- temperatureThe homogeneous solution was cooled
- washwashed with 1N NaOH (1×100 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-fddecac2ec004fb285028b74eb0ac7d7
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09193736B2
反応ノート
読み込み中…