tert-Butyl (2-(methoxy(methyl)amino)-2-oxoethyl)carbamate → tert-butyl N-(2-oxopropyl)carbamate
반응식
CON(C)[C:4](=[O:14])[CH2:5][NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10].[CH3:16][Mg+].[Br-]>C1COCC1>[O:14]=[C:4]([CH3:16])[CH2:5][NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10]참가 물질
4
실험 절차
To a solution of tert-butyl 2-(methoxy(methyl)amino)-2-oxoethylcarbamate (4.36 g, 0.02 mol) in THF (50 mL) added MeMgBr (40 ml, 0.08 ol) at −78° C. The formed mixture was stirred overnight. The mixture was quenched with NH4Cl and extracted with EtOAc. The organic phase was separated, dried over anhydrous Na2SO4, concentrated and purified by column chromatography to give tert-butyl 2-oxopropylcarbamate (2.5 g, 72%). 1H NMR (400 MHz, CDCl3): δ=1.42 (s, 9H), 2.18 (s, 3H), 4.01 (s, 2H), 5.22 (s, 1H).
후처리
- customThe mixture was quenched with NH4Cl
- extractionextracted with EtOAc
- customThe organic phase was separated
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
- custompurified by column chromatography
출처 및 근거
- ORD 기록
- ord-ee14afc0a8d647029fc37246ce71ef5f
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08575156B2
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