関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 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 | Dichloromethane | HCID 6344 | — |
| 生成物 | Diethyl p-toluoylaminomalonate | HCID 17447783 | 94.2% |
反応手順
To a suspension of diethyl aminomalonate hydrochloride (20.95 g, 97.02 mmol) and dry CH2Cl2 (180 mL) was added triethylamine (29.7 mL, 213 mmol). After cooling to 0° C., a solution of p-toluoyl chloride (15 g, 97 mmol) and CH2Cl2 (25 mL) was added at a rate such that the reaction temperature remained less than 5° C. The reaction was stirred at room temperature for 1 hour, cooled to 0° C. and quenched with water (90 mL). The organic layer was separated and washed with water (2×100 mL), 10% HCl (2×100 mL), water (2×100 mL) and brine (100 mL). The resultant solution was dried (Na2SO4), filtered and concentrated to give the title compound (26.8 g, 94%) as a white solid: mp 98°-99° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05646168 |
|---|
| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-257568f684614d14905001349cf072f5 |
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| 出典メモ | uspto-grants-1997_07 |
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