Water → HCID 66935046、化合物
反応式
COC([CH:5]1[CH:11]([CH3:12])[C:10](=[O:13])[NH:9][C:8]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:7]=2[C:6]1=[O:19])=O.O>CN(C=O)C>[Cl:18][C:15]1[CH:16]=[CH:17][C:7]2[C:6](=[O:19])[CH2:5][CH:11]([CH3:12])[C:10](=[O:13])[NH:9][C:8]=2[CH:14]=1参加物
4
反応条件
- 温度
- 230 °C
実験手順
To a solution of 8-chloro-3-methyl-2,5-dioxo-2,3,4,5-tetrahydro-1H-benzo[b]azepine-4-carboxylic acid methyl ester (iii-i) (0.2 g, 0.7 mmol) in DMF (2 mL) was added H2O (0.3 mL) and the reaction mixture heated to 230° C. in a microwave reactor for 5 minutes. H2O (20 mL) was added to the reaction mixture and the resulting precipitate was filtered and washed with H2O. The solid was dried under reduced pressure at 40° C. for 16 h to afford iv-i (0.12 g, 77%) as a white solid: MS m/z=224 (M+H).
後処理
- filtrationthe resulting precipitate was filtered
- washwashed with H2O
- customThe solid was dried under reduced pressure at 40° C. for 16 h
- customto afford iv-i (0.12 g, 77%) as a white solid
出典と根拠
- ORDレコード
- ord-03c35031532b478eb67ccd5271bf4b9d
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07935694B2
反応ノート
読み込み中…