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Dichloromethane → Diethyl p-toluoylaminomalonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 4-Methylbenzoyl Chloride | HCID 13405 | — |
| 反応物 | Propanedioic acid, 2-amino-, 1,3-diethyl ester, hydrochloride (1:1) | HCID 3084143 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Diethyl p-toluoylaminomalonate | HCID 17447783 | 91.2% |
反応手順
Diethyl aminomalonate hydrochloride (20.5 g) was suspended into 180 ml of methylene chloride, and 29.4 g of triethylamine was added while cooling with ice-cold water. After 30-minute-stirring, 15 g of p-toluoyl chloride was added dropwise, and the mixture was stirred for 24 hours at room temperature. The reaction solution was washed with water, dilute hydrochloric acid, and water, dried over anhydrous magnesium sulfate and concentrated. To the residue was added isopropyl ether, and the resultant crystals were collected by filtration and dried to provide 25.9 g of the objective compound as white crystal. M.p. 101-102° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07144906B2 |
| 出典データセット | uspto-grants-2006_12 |
| ORD ID | ord-98bd880f558a4fcca0e0ecf3e3922321 |
| 出典メモ | uspto-grants-2006_12 |