참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chlorotrimethylsilane | HCID 6397 | — |
| 반응물 | Alpha-Aminobutyric Acid | HCID 6657 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Butyryl chloride | HCID 8855 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Butyrylaminobutyric acid | HCID 12408866 | — |
반응 단계
25.78 g of 2-aminobutyric acid (250 mmol) and 55.66 g (550 mmol) of triethylamine are dissolved in 250 ml of dichloromethane, and the solution is cooled to 0° C. 59.75 g (550 mmol) of trimethylsilyl chloride are added dropwise, and the solution is stirred at room temperature for 1 hour and at 40° C. for one hour. After cooling to −10° C., 26.64 g (250 mmol) of butyryl chloride are added dropwise, and the resulting mixture is stirred at −10° C. for 2 hours and at room temperature for one hour. With ice-cooling, 125 ml of water are added dropwise, and the reaction mixture is stirred at room temperature for 15 minutes. Aqueous sodium hydroxide solution is added to the organic phase, and the organic solvent is removed under reduced pressure. The residue is acidified and the precipitated solid is triturated once with water and twice with petroleum ether and dried under reduced pressure at 45° C. 29.1 g (67%) of a colorless solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07098207B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-46b5a06419784ab4aa0ab701d258a09a |
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| 출처 메모 | uspto-grants-2006_08 |
|---|