反応式
C[O-].[Na+].CC1C=CC(S(O[C:15]([C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:16][C:17]#[N:18])(=O)=O)=CC=1.Cl.[NH2:24][CH:25](C(OCC)=O)[C:26]([O:28][CH2:29]C)=[O:27]>CO>[NH2:18][C:17]1[CH:16]=[C:15]([C:19]([CH3:20])([CH3:21])[CH3:22])[NH:24][C:25]=1[C:26]([O:28][CH3:29])=[O:27]参加物
実験手順
To a stirred sodium methoxide solution (15% by weight, 80 mL total) was added drop-wise a solution of 1-cyano-3,3-dimethylbut-1-en-2-yl 4-methylbenzenesulfonate (10.0 g, 36 mmol) and diethyl aminomalonate hydrochloride salt (9.0 g, 43 mmol) in methanol (50 mL). After the addition was completed, the reaction was stirred at room temperature for 2 hours, the solvent was removed under vacuum and the crude product was dissolved in water and extracted with ethyl acetate. The combined organic layers was washed with brine, dried and the solvent removed under vacuum. The crude product was purified by column chromatography (silicagel, dichloromethane:methanol 95:5) to afford 2.4 g of the desired methyl 3-amino-5-tert-butyl-1H-pyrrole-2-carboxylate used as such in the next step.
後処理
- additionAfter the addition
- customthe solvent was removed under vacuum
- dissolutionthe crude product was dissolved in water
- extractionextracted with ethyl acetate
- washThe combined organic layers was washed with brine
- customdried
- customthe solvent removed under vacuum
- customThe crude product was purified by column chromatography (silicagel, dichloromethane:methanol 95:5)
出典と根拠
- ORDレコード
- ord-dbed93c467224da4b16a268bb97437de
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741479B2
関連ノート
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