Hydrochloric Acid → HCID 117824033、化合物
反応式
[Na].[CH:2]1([CH2:5][O:6][CH2:7][C:8](=O)[CH2:9][C:10]([O:12]CC)=O)[CH2:4][CH2:3]1.[NH2:16][C:17]([NH2:19])=[S:18].Cl>CCO>[CH:2]1([CH2:5][O:6][CH2:7][C:8]2[NH:19][C:17](=[S:18])[NH:16][C:10](=[O:12])[CH:9]=2)[CH2:4][CH2:3]1参加物
6
実験手順
Sodium (4.0 g, 172 mmol) was added to EtOH (80 mL) and stirred until all dissolved at 60° C. The solution was cooled down to rt and a solution of ethyl 4-(cyclopropylmethoxy)-3-oxobutanoate (15.7 g, 78.4 mmol) in EtOH (80 mL) was added, followed by thiourea (7.2 g, 94 mmol). The mixture was stirred under reflux conditions for 24 h. Hydrochloric acid (aq, 1 M) was added until pH˜4 and the mixture was concentrated in vacuo. The residue was purified by column chromatography on silica eluting with a gradient of EtOAc and DCM to give the title compound as a solid, 15.7 g (95%).
後処理
- dissolutionall dissolved at 60° C
- stirringThe mixture was stirred under reflux conditions for 24 h
- concentrationthe mixture was concentrated in vacuo
- customThe residue was purified by column chromatography on silica eluting with a gradient of EtOAc and DCM
出典と根拠
- ORDレコード
- ord-f9b6fd8e4fdc4b49abd347466603bf4c
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09439904B2
反応ノート
読み込み中…