Sodium Hydroxide → 3-(1-Isopropylphthalazin-6-yl)-4-methylbenzoic acid
反応式
[CH:1]([C:4]1[C:13]2[C:8](=[CH:9][C:10]([C:14]3[CH:15]=[C:16]([CH:22]=[CH:23][C:24]=3[CH3:25])[C:17]([O:19]CC)=[O:18])=[CH:11][CH:12]=2)[CH:7]=[N:6][N:5]=1)([CH3:3])[CH3:2].[OH-].[Na+]>O1CCCC1.CO>[CH:1]([C:4]1[C:13]2[C:8](=[CH:9][C:10]([C:14]3[CH:15]=[C:16]([CH:22]=[CH:23][C:24]=3[CH3:25])[C:17]([OH:19])=[O:18])=[CH:11][CH:12]=2)[CH:7]=[N:6][N:5]=1)([CH3:3])[CH3:2]参加物
5
実験手順
A solution of ethyl 3-(1-isopropylphthalazin-6-yl)-4-methylbenzoate (37.5 mg, 0.11 mmol) in tetrahydrofuran (0.3 mL) and methanol (0.15 mL) was treated with 1N aq. sodium hydroxide (0.28 mL, 0.28 mmol) and stirred at RT for 18 h. The reaction mixture was concentrated in vacuo and the residue was taken up in water. The pH was adjusted with 10% HCl solution to ˜7. The precipitate formed was collected via filtration and dried under high vacuum to afford the title compound as a maize-colored solid. MS (ES+): 307.2 (M+H)+.
後処理
- concentrationThe reaction mixture was concentrated in vacuo
- customThe precipitate formed
- filtrationwas collected via filtration
- customdried under high vacuum
出典と根拠
- ORDレコード
- ord-a7e68c960a7c40c980802abcf80c3f6b
- 出典データセット
- uspto-grants-2010_07
- 特許番号
- US07759337B2
反応ノート
読み込み中…