Acetic Acid → HCID 69003844、化合物
反応式
CO[CH2:3][CH2:4][O:5][CH3:6].[C:7](/[C:9](/[C:24]1[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=1)=[CH:10]\[N:11]([CH2:19][C:20]([O:22][CH3:23])=[O:21])CCC(OCC)=O)#[N:8].[CH2:30]1[CH2:40]CN2C(=NCCC2)CC1.C(O)(=[O:43])C>>[NH2:8][C:7]1[C:9]([C:24]2[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=2)=[C:10]([CH2:40][CH2:30][C:6]([O:5][CH2:4][CH3:3])=[O:43])[NH:11][C:19]=1[C:20]([O:22][CH3:23])=[O:21]参加物
5
反応条件
- 温度
- 60 °C
実験手順
To an ethylene glycol dimethyl ether (50 mL) solution of ethyl 3-{((1Z)-2-cyano-2-(3-pyridyl)vinyl)[(methoxycarbonyl)methyl]amino}propanate (6.236 g) was added 1,8-diazabicyclo[5,4,0]-7-undecene (3.590 g), and the mixture was stirred at 60° C. overnight. The reaction solution was cooled to room temperature and neutralized with acetic acid, and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=1/5), to obtain the title compound (4.380 g, yield 70%). The NMR data and ESI/MS data of the compound are given below.
後処理
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by column chromatography on silica gel (hexane/ethyl acetate=1/5)
出典と根拠
- ORDレコード
- ord-41352add16f3403abe5a7a49ecec2673
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07557113B2
反応ノート
読み込み中…