Sodium → HCID 59558452、化合物
反応式
[CH2:1]([O:3][C:4](=[O:15])[CH2:5][C:6]([NH:8][C:9]1([CH2:12][CH:13]=[O:14])[CH2:11][CH2:10]1)=[O:7])C.[Na]>C1(C)C=CC=CC=1.CO>[CH3:1][O:3][C:4]([CH:5]1[C:13](=[O:14])[CH2:12][C:9]2([CH2:11][CH2:10]2)[NH:8][C:6]1=[O:7])=[O:15]参加物
5
実験手順
N-[1-(2-Oxo-ethyl)-cyclopropyl]-malonamic acid ethyl ester (200 mg; 0.823 mmol) in toluene (3 ml) is added to a solution of sodium (18.9 mg; 0.823 mmol) in MeOH (1 ml). The reaction mixture is refluxed for 45 minutes, poured on water and washed with TBME. The aqueous phase is acidified with 2N HCl (0.2 ml) and evaporated to dryness to yield the title compound as yellow resin (162 mg; 100%). 1H-NMR (400 MHz; DMSO-d6): 8.39 (s, 1H); 3.73 (s, 3H); 3.18 (s, 1H); 2.48 (s, 2H); 0.76 (m, 2H); 0.64 (m, 2H). MS (m/z) ES+: 198 (MH+).
後処理
- temperatureThe reaction mixture is refluxed for 45 minutes
- additionpoured on water
- washwashed with TBME
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-25e4654fb79d49e3adb26716aec926d2
- 出典データセット
- uspto-grants-2010_11
- 特許番号
- US07838674B2
反応ノート
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