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 solution 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 organic phase was washed with water, dried over MgSO4 and concentrated in vacuo. Purification with CC (KP-SIL™ from Biotage) using Hept/EtOAc (95/5 to 30/70) gives the desired compound as white solid.
後処理
- customThe solvent was evaporated off
- customthe residue partitioned between DCM and water
- washThe organic phase was washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customPurification with CC (KP-SIL™ from Biotage)
出典と根拠
- ORDレコード
- ord-f60fc32ce735477489d4915e23c9c01a
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09409917B2
反応ノート
読み込み中…