Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chlorodifluoromethane → 1-[1-(Difluoromethoxy)naphthalen-2-yl]ethan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chlorodifluoromethane | HCID 6372 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1'-Hydroxy-2'-acetonaphthone | HCID 69733 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 1-[1-(Difluoromethoxy)naphthalen-2-yl]ethan-1-one | HCID 2360828 | — |
반응 단계
10 g of 1-hydroxy-2-acetylnaphthalene are dissolved in 60 ml of dioxane, and 30 ml of 30% sodium hydroxide solution are added. At a temperature of from 70° C. to 80° C., difluorochloromethane (Freon 22) is introduced until no further absorption is observed. The dioxane phase is then decanted, the NaOH phase is washed with dioxane, the dioxane phase is decanted, and the combined dioxane solutions are largely concentrated in vacuo using a rotary evaporator. Water is added to the residue, the mixture is extracted several times with diethyl ether, and the diethyl ether solution is dried over Na2SO4, filtered and concentrated by evaporation. The residue is recrystallised from diethyl ether/hexane. Yield: 4 g, m.p. 80°-81° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05468751 |
| 출처 데이터셋 | uspto-grants-1995_11 |
| ORD ID | ord-2b18abdb79884dd28e51164fd3827cd8 |
| 출처 메모 | uspto-grants-1995_11 |