Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethanol → 6-(3-Chlorobenzyl)-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 | Ethyl 2-(3-chlorophenyl)acetate | HCID 8063366 | — |
| 반응물 | 5-amino-1-cyclopentyl-1H-pyrazole-4-carboxamide | HCID 11701191 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6-(3-Chlorobenzyl)-1-cyclopentyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one | HCID 135482330 | — |
반응 단계
Under argon, 180 mg (0.91 mmol) of 5-amino-1-cyclopentyl-1H-pyrazole-4-carboxamide and 575 mg (2.72 mmol; 3 equiv.) of ethyl (3-chlorophenyl)acetate are introduced into 3.5 ml of absolute ethanol. At 0° C., 127 mg of sodium hydride (60% dispersion in mineral oil; 3.18 mmol; 3.5 equiv.) are slowly added in a countercurrent of argon. The resulting mixture is slowly warmed and stirred under reflux for 18 h. The mixture is worked up by adding 50 ml of water and 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 | US08158633B2 |
| 출처 데이터셋 | uspto-grants-2012_04 |
| ORD ID | ord-31b26db9e03744e59abc79ad8d68d153 |
| 출처 메모 | uspto-grants-2012_04 |