関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 反応物 | 2-Butynoic acid | HCID 68535 | — |
| 反応物 | 6-Amino-4-(3,4-dibromophenylamino)quinoline-3-carbonitrile | HCID 10158966 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-[4-[(3,4-dibromophenyl)amino]-3-cyano-6-quinolinyl]-2-butynamide | HCID 10299692 | 46.9% |
反応手順
Isobutyl chloroformate (0.984 g, 7.18 mmol) and N-methylmorpholine (0.725 g, 7.18 mmol) were added to an ice cold solution of 0.604 g (7.18 mmol) of 2-butynoic acid in 25 mL of tetrahydrofuran. After 10 min, a solution of 1.20 g (2.87 mmol) of 6-amino-4-[(3,4-dibromophenyl)amino]-3-quinolinecarbonitrile in 12 mL of tetrahydrofuran was added dropwise. After stirring overnight at 25° C., volatile material was removed and the residue was slurried in water and filtered. The crude product was washed with boiling EtOAC and ethanol and dried in vacuo(50° C.) to give 0.651 g of brown solid: mass spectrum (electrospray, m/e): M+H 485.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06002008 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-43e5ecd14e7c40488cc4dbae8980f022 |
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| 出典メモ | uspto-grants-1999_12 |
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