Sodium Azide → (E)-4-(4-azidobut-1-enyl)-1,2-dichlorobenzene
반응식
CS(O[CH2:6][CH2:7]/[CH:8]=[CH:9]/[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=1)(=O)=O.[N-:18]=[N+:19]=[N-:20].[Na+]>CN(C=O)C.CCOC(C)=O>[N:18]([CH2:6][CH2:7]/[CH:8]=[CH:9]/[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=1)=[N+:19]=[N-:20]참가 물질
5
실험 절차
To a solution of Intermediate 2C (1.3 g, 4.4 mmol) in DMF (7 mL) was added NaN3 (0.86 g, 13 mmol). The reaction mixture was stirred at rt for 16 h. The reaction mixture was diluted with EtOAc (100 mL). The organic layer was washed with 10% aqueous LiCl solution (3×200 mL), dried over Na2SO4 and dried in vacuo. The product was isolated by silica gel chromatography to obtain 570 mg (87% yield) of Intermediate 2D. HPLC/MS (Method C)RT=4.02 min, [M+Na]+ 263.2.
후처리
- washThe organic layer was washed with 10% aqueous LiCl solution (3×200 mL)
- dry with materialdried over Na2SO4
- customdried in vacuo
- customThe product was isolated by silica gel chromatography
출처 및 근거
- ORD 기록
- ord-254b620c16f8478fb2c6143a0616b293
- 출처 데이터셋
- uspto-grants-2015_02
- 특허 번호
- US08952180B2
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