Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 7-Phenylthio-1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 7-Bromo-3,6,6-trimethyl-1-pyridin-2-yl-5,7-dihydroindazol-4-one | HCID 4073986 | — |
| 반응물 | Sodium 2-thenoate | HCID 23672340 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | 7-Phenylthio-1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole | HCID 9820424 | 45% |
반응 단계
The solution of 7-bromo-1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole (0.6 g, 1.8 mmol), prepared as described in example 4, and sodium thiophenate (0.3 g, 2.24 mmol) in dry N,N-dimethylformamide (10 ml) was stirred at room temperature for about 5 hours and then poured into brine and extracted with dichloromethane. The combined organic layers were washed with brine, dried over sodium sulfate end evaporated. The residue was chromatographed on silica gel (cyclohexane:ethyl acetate=90:10) to give 0.3 g (45% yield) of the title compound as a colourless solid which crystallized on standing.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06716856B1 |
| 출처 데이터셋 | uspto-grants-2004_04 |
| ORD ID | ord-dba86186f0bb4c3aac923286a6fe568d |
| 출처 메모 | uspto-grants-2004_04 |