Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 5-(Ethylthio)carbonyloxy-1-methylpyrazol-4-yl 3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)phenyl ketone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Ethyl chlorothioformate | HCID 18056 | — |
| 반응물 | HCID 178496176 | HCID 178496176 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-(Ethylthio)carbonyloxy-1-methylpyrazol-4-yl 3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)phenyl ketone | HCID 87233556 | — |
반응 단계
The crude 5-hydroxy-1-methylpyrazol-4-yl 3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)phenyl ketone obtained in the above step (3) was dissolved in anhydrous THF (10 mL), and triethylamine (190 mg) and 96% S-ethyl chlorothiolformate (151 mg) were added, followed by stirring for 1 hour at room temperature. Ethyl acetate (200 mL) was added to the reaction mixture, and the mixture was washed twice with a saturated brine. The organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1) to obtain the desired product (250 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08030498B2 |
| 출처 데이터셋 | uspto-grants-2011_10 |
| ORD ID | ord-f40119f5ce2d4267976ee95a02dbe706 |
| 출처 메모 | uspto-grants-2011_10 |