Methyl iodide → Methyl 1-methyl-4-(methylsulfanyl)-1H-pyrrole-2-carboxylate
反応式
[C:1]([S:3][C:4]1[CH:5]=[C:6]([C:10]([O:12][CH3:13])=[O:11])[N:7]([CH3:9])[CH:8]=1)#N.CI.C[O-].[Na+]>CO>[CH3:13][O:12][C:10]([C:6]1[N:7]([CH3:9])[CH:8]=[C:4]([S:3][CH3:1])[CH:5]=1)=[O:11]参加物
5
実験手順
4-Cyanothio-2-methoxycarbonyl-1-methylpyrrole (2.8 g, 14.3 mmol) is dissolved in 50 ml of methanol under nitrogen. Methyliodide (1.25 ml, 20 mmol) is added followed by 1.08 g (20 mmole) of sodium methoxide. After stirring for about 30 minutes at room temperature, the reaction mixture is concentrated to a paste and then diluted with 100 ml of ethylether. The resulting precipitate is filtered off and the filtrate concentrated to give an oil which is distilled at 100° to 104° at 0.25 mm-Hg to afford 2.2 g (86%) of 2-methoxycarbonyl-4-methylthio-1-methylpyrrole.
後処理
- concentrationthe reaction mixture is concentrated to a paste
- additiondiluted with 100 ml of ethylether
- filtrationThe resulting precipitate is filtered off
- concentrationthe filtrate concentrated
- customto give an oil which
- distillationis distilled at 100° to 104° at 0.25 mm-Hg
出典と根拠
- ORDレコード
- ord-f1eb8c74659848ad9c68267343a919f7
- 出典データセット
- uspto-grants-1984_02
- 特許番号
- US04434175
反応ノート
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