참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,2,4-Triazolo(4,3-a)pyridin-3(2H)-one | HCID 81431 | — |
| 반응물 | Methyl 3-bromo-2-(bromomethyl)propanoate | HCID 140895 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-(3-Oxo-[1,2,4]triazolo[4,3-a]pyridin-2-ylmethyl)acrylic acid methyl ester | HCID 57927603 | — |
반응 단계
After dissolving 2H-[1,2,4]triazolo[4,3-a]pyridin-3-one (CAS 6969-71-7) (1.0 g) in N,N-dimethylformamide (50 ml), sodium hydride (60% in oil) (355 mg) was added while stirring on ice. After stirring for 20 minutes, methyl 3-bromo-2-(bromomethyl)propionate (2.11 ml) was added dropwise. Stirring was continued for 1 hour and 30 minutes, and then sodium hydride (60% in oil) (200 mg) was added and the mixture was stirred for 3 hours. Water was added to the reaction mixture, and extraction was performed with ethyl acetate. The organic layer was washed with water and brine in that order and then dried over anhydrous magnesium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified by NH silica gel column chromatography to obtain the title compound (400 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08252810B2 |
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| 출처 데이터셋 | uspto-grants-2012_08 |
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| ORD ID | ord-27aa4b6cbe6a4901ad71e4490bbf1562 |
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| 출처 메모 | uspto-grants-2012_08 |
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