Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 1-(4'-Methoxyphenyl)-1,4-dihydro-indeno[1,2-c] pyrazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Methoxyphenylhydrazine hydrochloride | HCID 2723904 | — |
| 반응물 | 1H-Inden-1-one, 2,3-dihydro-2-(hydroxymethylene)- | HCID 3764882 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 1-(4'-Methoxyphenyl)-1,4-dihydro-indeno[1,2-c] pyrazole | HCID 15319940 | — |
반응 단계
2-Hydroxymethylene inden-l-one (Example 1(ii) (a) (4.0 g; 25 mmol), p-methoxyphenyl hydrazine hydrochloride (Aldrich) (4.41 g; 25.25 mmol), 10 M hydrochloric acid (1 cm3) and ethanol (30 cm3), were heated under reflux, for 21 hours. After cooling, the mixture was concentrated in vacuo and the residue dissolved in dichloromethane, then washed with 2M NaOH, dried, filtered and concentrated in vacuo. Purification by column chromatography [Eluant: (dichloromethane: ethanol: ammonia (200:8:1)] Kugelrohr distillation (170° C.; 0.02 mmHg) and recrystallisation (ethanol) afforded needle shaped crystals, m.p. 102-103° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06130228 |
| 출처 데이터셋 | uspto-grants-2000_10 |
| ORD ID | ord-2d264ec5b08e4c85957d76acb20b40b8 |
| 출처 메모 | uspto-grants-2000_10 |