참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | Propanimidamide, 2,2-dimethyl-, hydrochloride (1:1) | HCID 2781880 | — |
| 생성물 | HCID 178431765 | HCID 178431765 | — |
반응 단계
A single-necked flask containing 80 ml of ethanol is cooled down to 0° C. by an ice bath, 4 g (55.6 mmoles) of sodium ethylate and 3.8 g (27.8 mmoles) of tert-butylcarbamidine hydrochloride are added. The reaction mixture is left to return to ambient temperature, then 5 ml (27.8 mmoles) of diethyl ester methylmalonate is added dropwise. Stirring is maintained at ambient temperature overnight. The ethanol is then condensed under reduced pressure (2 kPa). The crude product obtained is solubilized in a minimum amount of water (approximately 40 ml), then acidified at 0° C. with pure acetic acid until a pH comprised between 4 and 5 is achieved. The white precipitate formed is filtered, rinsed successively with water, ethyl ether and with pentane. Then the white powder obtained is dried over P2O5 under reduced pressure (0.2 kPa). 2.4 g of expected product is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07825119B2 |
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| 출처 데이터셋 | uspto-grants-2010_11 |
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| ORD ID | ord-e25f6e52b443442485b9bc72056c4704 |
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| 출처 메모 | uspto-grants-2010_11 |
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