Sodium Acetate → 3,5-Dichloro-2-cyanobenzyl acetate
反応式
Br[CH2:2][C:3]1[CH:10]=[C:9]([Cl:11])[CH:8]=[C:7]([Cl:12])[C:4]=1[C:5]#[N:6].[CH3:13][C:14]([O-:16])=[O:15].[Na+]>CC(O)=O>[C:14]([O:16][CH2:2][C:3]1[CH:10]=[C:9]([Cl:11])[CH:8]=[C:7]([Cl:12])[C:4]=1[C:5]#[N:6])(=[O:15])[CH3:13]参加物
4
反応条件
- 温度
- 100 °C
実験手順
To a soln. of 2-(bromomethyl)-4,6-dichlorobenzonitrile (15.1 mmol) in 30 mL AcOH was added NaOAc (75.7 mmol). The suspension was heated to 100° C. for 2 h. The solvent was evaporated off and the residue partitioned between DCM and water. The org. phase was washed with water, dried over MgSO4 and conc. in vacuo. Purification with CC (5-70% EtOAc/Hept) gives the desired compound as white solid.
後処理
- customThe solvent was evaporated off
- customthe residue partitioned between DCM and water
- washphase was washed with water
- dry with materialdried over MgSO4 and conc. in vacuo
- customPurification with CC (5-70% EtOAc/Hept)
出典と根拠
- ORDレコード
- ord-49248ed03b8441708d7f4efcba372914
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09388197B2
反応ノート
読み込み中…