tert-Butyl (2-(methoxy(methyl)amino)-2-oxoethyl)carbamate → tert-butyl N-(2-oxopropyl)carbamate
反応式
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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-ee14afc0a8d647029fc37246ce71ef5f
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08575156B2
反応ノート
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