Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethanol → 6-(Cyclohexylmethyl)-1-cyclopentyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Cyclohexaneacetic acid, methyl ester | HCID 139743 | — |
| 반응물 | 5-amino-1-cyclopentyl-1H-pyrazole-4-carboxamide | HCID 11701191 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6-(Cyclohexylmethyl)-1-cyclopentyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one | HCID 135407177 | — |
반응 단계
Under argon, 75 mg (039 mmol) of 5-amino-1-cyclopentyl-1H-pyrazole-4-carboxamide and 183 mg (1.16 mmol, 3 equiv.) of methyl cyclohexylacetate are introduced into 1.5 ml of absolute ethanol. At 0° C., 54 mg of sodium hydride (60% dispersion in mineral oil; L35 mmol, 15 equiv.) are slowly added in a countercurrent of argon. The resulting mixture is slowly heated and stirred under reflux for 18 h. For workup, 20 ml of water are added, and the mixture is extracted several times with ethyl acetate. The combined organic phases are dried over sodium sulfate and concentrated in vacuo. The crude product is purified by preparative HPLC.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08741907B2 |
| 출처 데이터셋 | uspto-grants-2014_06 |
| ORD ID | ord-b4f99a1e32184dcc8b2f023c3b1bc9c8 |
| 출처 메모 | uspto-grants-2014_06 |