Cesium carbonate → HCID 86717939、化合物
反応式
[NH2:1][C:2]1[C:7]([OH:8])=[C:6]([F:9])[CH:5]=[CH:4][N:3]=1.Br[CH2:11][C:12]1[C:17]([F:18])=[CH:16][CH:15]=[CH:14][C:13]=1[F:19].C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C>[F:18][C:17]1[CH:16]=[CH:15][CH:14]=[C:13]([F:19])[C:12]=1[CH2:11][O:8][C:7]1[C:2]([NH2:1])=[N:3][CH:4]=[CH:5][C:6]=1[F:9]参加物
5
反応条件
- 温度
- 50 °C
実験手順
55 mg (0.43 mmol) of 2-amino-4-fluoropyridin-3-ol Example 267A, 98 mg (0.47 mmol) of 2-(bromomethyl)-1,3-difluorobenzene and 308 mg (0.95 mmol) of caesium carbonate were initially charged in 1 ml of dry DMF and heated for 15 min in an oil bath warmed to 50° C. The mixture was then filtered off and purified by preparative HPLC (Method 9). This gave 70 mg of the title compound (64% of theory).
後処理
- temperatureheated for 15 min in an oil bath
- filtrationThe mixture was then filtered off
- custompurified by preparative HPLC (Method 9)
出典と根拠
- ORDレコード
- ord-dc380e3999a64bd69fe22150de8da738
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09126998B2
反応ノート
読み込み中…