反応式
Br[CH:2]([CH3:15])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:6]=1)=O.[NH2:16][C:17]1[N:22]=[CH:21][CH:20]=[CH:19][N:18]=1.C(=O)(O)[O-].[Na+]>CC(O)C>[CH3:15][C:2]1[N:16]=[C:17]2[N:22]=[CH:21][CH:20]=[CH:19][N:18]2[C:3]=1[C:5]1[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:6]=1参加物
実験手順
In a thermally controlled reactor, stir a mixture of 2-bromo-1-[4-(trifluoromethyl)phenyl]propan-1-one (500 g, 1.78 mol, 1 equiv), IPA (5 L), 2-aminopyrimidine (205 g, 2.13 mol, 1.2 equiv), and sodium bicarbonate (298.8 g, 3.55 mol, 2 equiv) at 80° C. for 18 hours. Cool the suspension, and concentrate in vacuo. Dilute the resulting mixture in DCM (5 L), and wash with brine (2 L). Re-extract the brine wash with DCM (2.5 L); combine all the organic phases; and dry over MgSO4; filter; and collect the filtrate. Concentrate the filtrate to dryness under reduced pressure, and slurry the resulting red gum in Et2O (1.5 L). Collect the resulting solid by filtrate, and air dry for 45 min to give the title compound as a fine, off white solid (108 g, 22% yield). MS (m/z) 278 (M+1).
後処理
- temperatureCool the suspension
- concentrationconcentrate in vacuo
- additionDilute the resulting mixture in DCM (5 L)
- washwash with brine (2 L)
- washRe-extract the brine wash with DCM (2.5 L)
- dry with materialand dry over MgSO4
- filtrationfilter
- customand collect the filtrate
- concentrationConcentrate the filtrate to dryness under reduced pressure
- customCollect the resulting solid by filtrate, and air
- customdry for 45 min
出典と根拠
- ORDレコード
- ord-705882bb16214e3b947072f0284455fb
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08648200B2
関連ノート
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