참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Methyl chloroformate | HCID 6586 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | (-)-Valerenic acid | HCID 6440940 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (-)-Valerenic acid | HCID 6440940 | — |
| 생성물 | Valerenic acid amide | HCID 46835834 | — |
반응 단계
Valerenic acid (18.9 mg, 0.0807 mmol) was dissolved in THF (3 mL) and cooled to 0° C. Triethylamin (12.0 μL, 8.76 mg, 0.0866 mmol) and methyl chloroformate (97%, 8.5 μL, 9.36 mg, 0.0862 mmol) were added. After stirring for 1 hour the resulting solution was treated with aqueous ammonia (25% 25 μL, 5.5 mg, 0.3230 mmol). After 30 minutes the reaction mixture was warmed to room temperature and stirred for an additional hour. Then the mixture was filtrated and the filtrate concentrated in vacuo. Purification by chromatography (pure diethylether to diethylether/EtOAc 1/1) provided 6.6 mg Valerenic acid and 11.2 mg of Valerenic acid amide as white solid with 92% yield based on recovered starting material.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08809395B2 |
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| 출처 데이터셋 | uspto-grants-2014_08 |
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| ORD ID | ord-f330f0febe7b45ef92818f4f1a40913a |
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| 출처 메모 | uspto-grants-2014_08 |
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