関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-Pyrrolidinebutanoic acid | HCID 14855681 | — |
| 反応物 | HCID 178424209 | HCID 178424209 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | HCID 178424210 | HCID 178424210 | — |
反応手順
To a suspension of 4-pyrrolidin-1-yl-butyric acid (118.0 mg, 0.8 mmol, 1.5 eq) in 1,2-dichloroethane (3 mL), N,N′-carbonyldiimidazole (113.0 mg, 0.7 mmol, 1.4 eq) was added and the mixture was stirred at room temperature for 1 hour, then N,N-diisopropyl ethyl amine (87 μL, 0.5 mmol, 1.0 eq) was added and the mixture was stirred at room temperature for further 1 hour until complete dissolution of the suspension. 4-Methyl-5-o-tolyl-2H-pyrazol-3-ylamine (93.5 mg, 0.5 mmol, 1.0 eq) was added and the reaction was stirred for 18 hours, then at 50° C. for 1 day, until the conversion of the less stable ring nitrogen-acylated isomer to the title compound was observed (as monitored by LC-MS). The solvent was removed under reduced pressure, the crude was purified by SiO2 column to give 44.0 mg of the title compound (yield: 27%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08163729B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-cbed115632004c539c8d102b4adc631c |
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| 出典メモ | uspto-grants-2012_04 |
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