Sodium Acetate → 3,5-Dichloro-2-cyanobenzyl acetate
반응식
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]참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-f60fc32ce735477489d4915e23c9c01a
- 출처 데이터셋
- uspto-grants-2016_08
- 특허 번호
- US09409917B2
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