Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2-[(3,5-Dimethylphenyl)sulfonyl]-6-fluorobenzenecarbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile | HCID 10848751 | — |
| 반응물 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-[(3,5-Dimethylphenyl)sulfonyl]-6-fluorobenzenecarbonitrile | HCID 486357 | 65% |
반응 단계
2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile (Example 18) (1.0 g 3.9 mmol) was dissolved in 100 ml of methanol. A solution of OXONE®.dagger. (5.26 g, 8.6 mmol) in 30 ml of water was added dropwise with stirring. After stirring 1 h, another 1.5 equivalents of OXONE® (3.60 g 5.9 mmol) was added. The reaction was stirred for 18 h. The solid was removed by vacuum filtration and washed with 200 ml of methanol, then with 2×60 ml of acetone. The filtrate was concentrated to dryness and chromatographed on silica gel (flash; Hex/EtOAc 1:1) to provide 0.73 g (65%) of 2-[(3,5-dimethylphenyl)sulfonyl]-6-fluorobenzonitrile: mp 167°-168° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05723452 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-3a63765ce57f4be88697886cd8f75569 |
| 출처 메모 | uspto-grants-1998_03 |