関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Pyrrolidinone, (4-aminophenyl)- | HCID 676146 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Benzyl 4-(2-oxo-1-pyrrolidinyl)phenylcarbamate | HCID 7686496 | 73.8% |
反応手順
4.27 g (25.03 mmol) of benzyl chloroformate are slowly added to 4 g (22.7 mmol) of 1-(4-aminophenyl)pyrrolidin-2-one and 3.6 ml (28.4 mmol) of N,N-dimethylaniline in 107 ml of tetrahydrofuran at −20° C. The mixture is stirred at −20° C. for 30 minutes and then allowed to reach room temperature. 0.5 l of ethyl acetate is added, and the organic phase is washed with 0.5 l of saturated NaCl solution. The removed organic phase is dried with MgSO4, and the solvent is evaporated in vacuo. The residue is triturated with diethyl ether and filtered off with suction. 5.2 g (73.8% of theory) of benzyl 4-(2-oxo-1-pyrrolidinyl)phenylcarbamate are obtained as pale beige crystals with a melting point of 174° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07767702B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-b678ad7d47524d1ab57465d1e6ea7d61 |
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| 出典メモ | uspto-grants-2010_08 |
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