Monobenzone → 5-(p-Hydroxyphenoxy)pyrimidine
反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1C=CC=CC=1.BrC1[CH:18]=[N:19][CH:20]=[N:21]C=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C.O>[OH:15][C:12]1[CH:11]=[CH:10][C:9]([O:8][C:1]2[CH:2]=[N:21][CH:20]=[N:19][CH:18]=2)=[CH:14][CH:13]=1参加物
6
反応条件
- 温度
- 120 °C
実験手順
To 1.00 g (4.99 mmol) 4-(benzyloxy)phenol and 794 mg (4.99 mmol) 5-bromo-pyrimidine in 5 mL DMF are added 3.25 g (9.99 mmol) Cs2CO3 and the reaction mixture is stirred at 120° C. for 6 h in a microwave oven. Then the reaction mixture is diluted with water and extracted with EtOAc. The organic layer is dried with Na2SO4 and the solvent is removed in vacuo. The residue is purified by HPLC (MeOH/H2O/NH3).
後処理
- extractionextracted with EtOAc
- dry with materialThe organic layer is dried with Na2SO4
- customthe solvent is removed in vacuo
- customThe residue is purified by HPLC (MeOH/H2O/NH3)
出典と根拠
- ORDレコード
- ord-e7978093a2dc4120954dbcd795fa8f7e
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08835472B2
反応ノート
読み込み中…