참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Butyryl chloride | HCID 8855 | — |
| 반응물 | Ethyl 2-amino-3-mercaptopropanoate hydrochloride | HCID 6432754 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl 2-butyramido-3-mercaptopropanoate | HCID 57989348 | — |
반응 단계
Triethylamine (4.5 mL) was added to a suspension of ethyl 2-amino-3-mercaptopropanoate hydrochloride (5 g) in DCM (50 mL). The resulting mixture was cooled in an ice/salt bath and butyryl chloride (3.3 mL) was added dropwise. The resulting mixture was allowed to warm to RT and stirred overnight. The reaction was quenched with saturated sodium bicarbonate solution (50 mL) and the layers separated. The aqueous phase was extracted with DCM (2×100 mL). The combined organic solutions were washed with brine (100 mL), dried over sodium sulphate, filtered and evaporated. The resulting white solid was purified by silica gel chromatography eluting with 4:1 to 1:1 isohexane:ethyl acetate gradient. The fractions containing product were combined and evaporated to give the subtitled compound as a white solid. Yield 3 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08148373B2 |
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| 출처 데이터셋 | uspto-grants-2012_04 |
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| ORD ID | ord-4bdedd386eb34d1aaa00c78079616978 |
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| 출처 메모 | uspto-grants-2012_04 |
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