Sodium Azide → 3-Azido-4-oxo-pentanoic acid methyl ester
반응식
[CH3:1][O:2][C:3](=[O:10])[CH2:4][CH:5](Br)[C:6](=[O:8])[CH3:7].[N-:11]=[N+:12]=[N-:13].[Na+]>CN(C=O)C.O>[CH3:1][O:2][C:3](=[O:10])[CH2:4][CH:5]([N:11]=[N+:12]=[N-:13])[C:6](=[O:8])[CH3:7]참가 물질
5
실험 절차
To a solution of 2.23 g (10.67 mmol) of 3-bromo4-oxo-pentanoic acid methyl ester in 11 mL of DMF at 0° C. was added 690 mg (10.67 mmol) of sodium azide. After warming to RT over 2.5 h, the reaction was diluted with water and extracted with diethyl ether/hexane (1:1). The layers were separated, the organics dried (Na2SO4), and the solvent removed in vacuo. The residue was purified by silica gel chromatography using diethyl ether/hexane (gradient of 1:4 to 2:3) to give 1.07 g (58% yield ) of the title compound: low resolution MS (FAB) m/e 172 (MH+).
후처리
- extractionextracted with diethyl ether/hexane (1:1)
- customThe layers were separated
- dry with materialthe organics dried (Na2SO4)
- customthe solvent removed in vacuo
- customThe residue was purified by silica gel chromatography
출처 및 근거
- ORD 기록
- ord-cd3907783d144dc1a3249b8e780e97f9
- 출처 데이터셋
- uspto-grants-2001_09
- 특허 번호
- US06294580B1
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