Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylhydantoin → 3-[4-(4-Pyridylthio)butyl]-5,5-dimethylhydantoin
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylhydantoin | HCID 6491 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | 4-(4-Chlorobutylthio)pyridine | HCID 15816978 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-[4-(4-Pyridylthio)butyl]-5,5-dimethylhydantoin | HCID 19079098 | 56.8% |
반응 단계
To a solution of 2.56 g (20 mmol) of 5,5-dimethylhydantoin and 4.03 g (20 mmol) of 4-(4-chlorobutylthio)pyridine in 20 ml of N,N-dimethylformamide, 3.00 ml (20 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene was added, and the mixture was stirred at room temperature for 43 hours, followed by further stirring at 70° C. for 10 hours. Ethyl acetate was added to the reaction mixture, and the mixture was washed three times with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/ethanol =10:1) to give 3.33 g of the desired compound (56.8% yield, colorless crystals).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05246948 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-223b53ba401c4783b307cafc7579f4f4 |
| 출처 메모 | uspto-grants-1993_09 |