참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | Benzyl-N-(1-cyanoethyl)glycine hydrochloride | HCID 68560147 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | Benzyl 2-[3,5-dichloro-2-methyl-6-oxo-1(6H)-pyrazinyl]acetate | HCID 10663926 | 55% |
반응 단계
A stirred mixture of oxalyl chloride (5.3 mL, 60 mmol) and benzyl-N-(1-cyanoethyl)glycine hydrochloride (3.82 g, 15 mmol), as prepared in the preceding step, in 1,2-dichlorobenzene (30 mL) was heated to 100° C. overnight. The solvent was evaporated in vacuo and the residue was purified by flash column chromatography (20-30% ethyl acetate in hexane) to give a solid. 10% Ethyl acetate in hexane (100 mL) was added and the solid was collected to give the title compound as an orange crystalline solid (2.7 g, 55%). 1H-NMR (300 MHz, CDCl3) δ 7.38 (m, 5H), 5.24 (s, 2H), 4.89 (s, 2H), 2.34 (S, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06514978B2 |
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| 출처 데이터셋 | uspto-grants-2003_02 |
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| ORD ID | ord-1d1ebf3e543c46028fe8b12b982e5d4e |
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| 출처 메모 | uspto-grants-2003_02 |
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