Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitric Acid → Thiomorpholine, 4-(2,6-difluoro-4-nitrophenyl)-, 1,1-dioxide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Pnu-288034 | HCID 9931003 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | Thiomorpholine, 4-(2,6-difluoro-4-nitrophenyl)-, 1,1-dioxide | HCID 9922094 | 94.2% |
반응 단계
To a suspension of the product of example 1 (300 g, 1.21 mol) in 3 L of acetic acid, nitric acid (255 mL, ca. 6 mol, fuming, 90%) is added over 30 min at room temperature. Yellow precipitate is formed within minutes and increases over time. The reaction is kept at room temperature for 18 hours, before it is poured into 6 L of water. After stirred for 2 hours, the yellow suspension is filtered. The precipitate is washed with water (1.5 L×3) and EtOH (0.5 L×2) and dried in oven at 50° C. overnight to give 333 g (94%) of the title compound as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06605609B2 |
| 출처 데이터셋 | uspto-grants-2003_08 |
| ORD ID | ord-005797f02363405c9b410f8b0a949391 |
| 출처 메모 | uspto-grants-2003_08 |