Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Toluenesulfonyl chloride → 1-(toluene-4-sulfonyl)-1H-pyrazole-4-carboxylic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | ethyl 1H-pyrazole-4-carboxylate | HCID 142179 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ammonium Chloride | HCID 25517 | — |
| 생성물 | 1-(toluene-4-sulfonyl)-1H-pyrazole-4-carboxylic acid ethyl ester | HCID 21628277 | — |
반응 단계
To a solution of ethyl 1H-pyrazole-4-carboxylate (4.50 g, 32.11 mmol) in THF was added 60% NaH (1.60 g, 40.00 mmol) in mineral oil. After 20 minutes, p-toluenesulfonyl chloride was added. After 3 hours, the mixture was diluted with saturated aqueous NH4Cl and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 30-50% ethyl acetate in heptane. The major fractions were combined and the solvent was concentrated in vacuo to afford 1-(toluene-4-sulfonyl)-1H-pyrazole-4-carboxylic acid ethyl ester.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08063065B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-c6c1caf4f0554cc580b27e0f9d6a773a |
| 출처 메모 | uspto-grants-2011_11 |