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Dimethylformamide dimethyl acetal → Ethyl 2-(5-chloro-2-methylbenzoyl)-3-(dimethylamino)acrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | Ethyl 3-(5-chloro-2-methylphenyl)-3-oxopropanoate | HCID 58063452 | — |
| 生成物 | Ethyl 2-(5-chloro-2-methylbenzoyl)-3-(dimethylamino)acrylate | HCID 66677099 | 34.2% |
反応手順
A solution of ethyl 3-(5-chloro-2-methylphenyl)-3-oxopropanoate (28.4 mmol) in 1,1-dimethoxy-N,N-dimethylmethanamine (10.0 mL, 75.3 mmol, 2.6 equiv) was heated at 90° C. After 3 hours, the reaction mixture was concentrated in vacuo, and the resultant residue was purified by flash column chromatography on silica gel (0 to 80% ethyl acetate in dichloromethane) to yield 2.87 g (34%) of ethyl 2-(5-chloro-2-methylbenzoyl)-3-(dimethylamino)acrylate. LCMS (ESI) m+H=296.3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08637526B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-f4b37a4b0eb74adbb5a5bd6de3382c84 |
| 出典メモ | uspto-grants-2014_01 |