Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfoxide → 2-(2-Hydroxy-5-nitrobenzyl)-5-methoxy-1-(4-methoxybenzenesulphonyl)-1,2-dihydroindazol-3-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2-(Chloromethyl)-4-nitrophenol | HCID 76305 | — |
| 반응물 | 5-methoxy-1H-indazol-3-yl 4-methoxybenzenesulphonate | HCID 15429047 | — |
| 생성물 | 2-(2-Hydroxy-5-nitrobenzyl)-5-methoxy-1-(4-methoxybenzenesulphonyl)-1,2-dihydroindazol-3-one | HCID 9805385 | — |
반응 단계
5.01 g (15 mmol) of 5-methoxy-1H-indazol-3-yl 4-methoxybenzenesulphonate are dissolved in 70 ml of DMSO and treated in portions with 1.5 g (37.5 mmol) of sodium hydride (60 percent). After stirring for 2 hours, a solution of 2.81 g (15 mmol) of 2-hydroxy-5-nitrobenzyl chloride in 25 ml of DMSO is added dropwise and the mixture is stirred at 90-100° C. for 3 hours. After cooling, 400 ml of water are added, and the mixture is stirred for 3 hours and extracted three times with 400 ml of ethyl acetate. The combined organic phases are washed with 100 ml of water, dried over sodium sulphate, distilled to dryness in vacuo and the residue is recrystallized from ethanol.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06180637B2 |
| 출처 데이터셋 | uspto-grants-2001_01 |
| ORD ID | ord-c071f75f633949b28c254c8a60b8ebe9 |
| 출처 메모 | uspto-grants-2001_01 |