Potassium Iodide → Glycine, N-(2,2-difluoroethyl)-, ethyl ester
反応式
[F:1][CH:2]([F:5])[CH2:3][NH2:4].Br[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].[I-].[K+].C(N(C(C)C)CC)(C)C>C(#N)C>[F:1][CH:2]([F:5])[CH2:3][NH:4][CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9]参加物
6
実験手順
2,2-difluoroethylamine (4.0 g) was added to a suspension of ethyl bromoacetate (5.4 mL), potassium iodide (0.82 g), diisopropylethylamine (9.8 mL) in acetonitrile (100 mL) and the mixture was stirred at RT for 25 h. The mixture was concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel to afford the sub-title compound (7.0 g) as a colorless oil; 1H NMR (300 MHz, CDCl3); 5.82 (1H, tt), 4.18 (2H, q), 3.46 (2H, s), 3.00 (2H, dt), 1.26 (3H, t).
後処理
- concentrationThe mixture was concentrated under reduced pressure
- customThe residue was purified by flash column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-b053c74e468b4549b3254fe9cae52beb
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09376398B2
反応ノート
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