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Magnesium orthosilicate → 2-Cyano-3dimethylamino-1-thien-3-ylpropen-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Magnesium orthosilicate | HCID 66225 | — |
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | 5-(Thiophen-3-yl)isoxazole | HCID 18516886 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Cyano-3dimethylamino-1-thien-3-ylpropen-1-one | HCID 29943485 | 56.5% |
反応手順
A mixture of 41.2 g of 5-(3-thienyl)isoxazole and 36.0 g of dimethylformamide dimethylacetal, under nitrogen, is heated on a stream bath for 4 hours. The reaction is concentrated in vacuo to give a viscous oil which solidified. The residue is dissolved in methylene chloride and passed thru a short column of hydrous magnesium silicate. On cooling, 31.76 g of the desired product is obtained, mp 118°-119°, CI-MS:m/z 206(M30). Concentrating in vacuo the methylene chloride gives an additional 20.2 g of product. (Total recovered 51.96 g, 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05059709 |
| 出典データセット | uspto-grants-1991_10 |
| ORD ID | ord-c173186a7e67482f8013b66cca805112 |
| 出典メモ | uspto-grants-1991_10 |