反応式
[CH3:1][N:2]([CH3:18])[CH:3]1[CH2:7][N:6]([C:8](=[O:17])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)[NH:5][CH2:4]1.[CH3:19][S:20]([C:23]1[N:28]=[C:27]([C:29](Cl)=[O:30])[CH:26]=[CH:25][N:24]=1)(=O)=O.[OH-].[Na+]>ClCCl>[CH3:18][N:2]([CH3:1])[CH:3]1[CH2:7][N:6]([C:8](=[O:17])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)[N:5]([C:29]([C:27]2[CH:26]=[CH:25][N:24]=[C:23]([S:20][CH3:19])[N:28]=2)=[O:30])[CH2:4]1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 1-(4-dimethylamino-pyrazolidin-1-yl)-2-(4-fluorophenyl)-ethanone, 22, (2.5 g, 10 mmol) in dichloromethane (20 mL) is added 2-methylsulfonyl-pyrimidine-4-carbonyl chloride (3.7 g, 20 mmol) followed by dropwise addition of a 1.0 N aqueous solution of sodium hydroxide (35 mL). The mixture is vigorously stirred at room temperature for 12 hours. The reaction is diluted with dichloromethane (100 mL) and washed with water (100 mL). The aqueous layer is back-extracted with dichloromethane (100 mL). The combined organic layers are washed with a saturated aqueous solution of sodium bicarbonate (100 mL) and brine (100 mL), dried, filtered and concentrated in vacuo. The resulting crude material is purified over silica (1:1 hexane/ethyl acetate to 100% ethyl acetate) to afford the desired product.
後処理
- washwashed with water (100 mL)
- extractionThe aqueous layer is back-extracted with dichloromethane (100 mL)
- washThe combined organic layers are washed with a saturated aqueous solution of sodium bicarbonate (100 mL) and brine (100 mL)
- customdried
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe resulting crude material is purified over silica (1:1 hexane/ethyl acetate to 100% ethyl acetate)
出典と根拠
- ORDレコード
- ord-82ece23e4b9a48208a1fafdf7af0877e
- 出典データセット
- uspto-grants-2004_05
- 特許番号
- US06730668B2
関連ノート
読み込み中…