Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → ethyl 5-(2-hydroxy-2-methylpropyl)-1-propyl-1H-pyrazole-3-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Diethyl Oxalate | HCID 7268 | — |
| 반응물 | Hydrazine, propyl-, ethanedioate (1:1) | HCID 96079 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | ethyl 5-(2-hydroxy-2-methylpropyl)-1-propyl-1H-pyrazole-3-carboxylate | HCID 66781950 | — |
반응 단계
To a solution of sodium tert-butoxide dissolved in ethanol (71 mL) was added diethyl oxalate (16.1 g, 110 mmol) followed by the material obtained in Part A (18.8 g, 100 mmol). The reaction was stirred 30 minutes at ambient temperature before cooling to 0° C. and adding acetic acid (100 mL) and propylhydrazine oxalate (16.4 g, 100 mmol). The reaction was allowed to warm to ambient temperature and stirred for 19 hours. The solvent was removed under reduced pressure. The resulting brown oil was purified by automated flash chromatography (AnaLogix, eluting with a gradient of 50-75% ethyl acetate in hexanes) to provide 9.6 g of ethyl 5-(2-hydroxy-2-methylpropyl)-1-propyl-1H-pyrazole-3-carboxylate as a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08138173B2 |
| 출처 데이터셋 | uspto-grants-2012_03 |
| ORD ID | ord-0beb1909aaac4e39a96bf49c09c5c581 |
| 출처 메모 | uspto-grants-2012_03 |