Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 6-Hydroxy-2,4,4-trimethyl-3,4-dihydro-2H-naphthalen-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Hydrogen Cyanide | HCID 768 | — |
| 반응물 | Sodium Cyanide | HCID 8929 | — |
| 반응물 | 6-methoxy-2,4,4-trimethyl-3,4-dihydro-2H-naphthalen-1-one | HCID 21107233 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 6-Hydroxy-2,4,4-trimethyl-3,4-dihydro-2H-naphthalen-1-one | HCID 21107231 | — |
반응 단계
A solution 6-methoxy-2,4,4-trimethyl-3,4-dihydro-2H-naphthalen-1-one (described in Journal of Pharmaceutical Sciences, 1970, 59(6), p 869-870, Floyd et al. incorporated herein by reference; 1.2 g, 5.5 mmol) and sodium cyanide (2 g, 41 mmol) in anhydrous dimethylsulfoxide (15 mL) was heated at 230° C. for 24 h under argon. The reaction mixture was then cooled to ambient temperature, poured into ice and acidified (Caution! Hydrogen cyanide evolution!) with dilute hydrochloric acid and extracted with ethyl acetate (×2). The combined organic extract was washed with brine (×1), dried over anhydrous sodium sulfate, filtered and evaporated to afford the title compound, which was used as such for the next step (1 g, 89%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07638648B2 |
| 출처 데이터셋 | uspto-grants-2009_12 |
| ORD ID | ord-16087d2915e34560b3b233118cdcaed0 |
| 출처 메모 | uspto-grants-2009_12 |