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4-Aminobenzonitrile → 1-(4-Cyanophenyl)-2-oxopyrrolidine-3-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminobenzonitrile | HCID 13396 | — |
| 反応物 | 6,6-Dimethyl-5,7-dioxaspiro(2.5)octane-4,8-dione | HCID 79720 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(4-Cyanophenyl)-2-oxopyrrolidine-3-carboxylic acid | HCID 66831830 | 36% |
反応手順
A mixture of 6,6-dimethyl-5,7-dioxaspiro[2.5]octane-4,8-dione (0.500 g, 2.94 mmol) and 4-aminobenzonitrile (1.04 g, 8.82 mmol) in ethanol (3 mL) was irradiated in a microwave oven for 3 minutes at 100° C. The solution was concentrated under reduced pressure and the residue was dissolved in a solution of sodium hydroxide 6N, washed with dichloromethane, acidified with a solution of sodium hydrogen phosphate (1M) to pH=2, extracted with ethyl acetate dried and concentrated under reduced pressure to yield 0.240 g (36%) of a brown solid, which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434722B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-f7052addfd7b40a1801b391e36511771 |
| 出典メモ | uspto-grants-2016_09 |