Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 2243767생성일: 2026년 10월 26일
Acetonitrile → 3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide
https://huagongshe.com/reaction/2243767
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | 3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide | HCID 11950263 | — |
| 반응물 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide | HCID 59207990 | — |
반응 단계
To a stirring suspension of Oxone (817.96 g, 1.33 mole, 3 eq) in water (2142 mL, 10 vol) was added 3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide (214.21 g 0.443 mole, 1 eq) suspended in acetonitrile (4284 mL). The resulting mixture was stirred at ambient temperature overnight. The mixture was then filtered and the residue stirred sequentially with 5% sodium metabisulfite (2×3000 mL) and water (1×300 mL). The filtrate from the reaction mixture was then diluted with water (2142 mL, 10 vol). The solid that formed was then collected by filtration. The solid was washed well with water then dried at the pump to yield the title compound. LC-MS m/z 516 (M+H)+, 2.77 min (ret time). It was used without further purification although corresponding sulfoxide was present (about 10%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07674789B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_03 |
|---|
| ORD ID | ord-76886ac03f234014bb68a8eca88cfe8d |
|---|
| 출처 메모 | uspto-grants-2010_03 |
|---|