Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 3-(1-Hydroxy-2,2,2-trifluoro-1-trifluoromethylethyl)-2-methyl-7-nitrobenzo[b]furan
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Hexafluoroacetone | HCID 12695 | — |
| 반응물 | Hexafluoroacetone trihydrate | HCID 36719 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 반응물 | 2-Methyl-7-nitrobenzofuran | HCID 13201897 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-(1-Hydroxy-2,2,2-trifluoro-1-trifluoromethylethyl)-2-methyl-7-nitrobenzo[b]furan | HCID 86753553 | — |
반응 단계
Into a mixture of 2-methyl-7-nitrobenzo[b]furan (200 mg) and aluminum chloride (301 mg) in dichloromethane was passed hexafluoroacetone gas which was made from hexafluoroacetone trihydrate (4.7 ml) and conc. sulfuric acid (15 ml). The mixture was stirred at ambient temperature for 4 hours and then, cooled to 4° C. To the mixture was added 1N-hydrochloric acid dropwise. The organic layer was separated, washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel and the obtained oil was crystallized from n-hexane to give 3-(1-hydroxy-2,2,2-trifluoro-1-trifluoromethylethyl)-2-methyl-7-nitrobenzo[b]furan (265 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05858995 |
| 출처 데이터셋 | uspto-grants-1999_01 |
| ORD ID | ord-9ad3bf85b765418e9a85d1c8f96c856a |
| 출처 메모 | uspto-grants-1999_01 |