HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 21107232, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Hydrogen Cyanide | HCID 768 | — |
| Reactant | Sodium Cyanide | HCID 8929 | — |
| Reactant | HCID 22218197 | HCID 22218197 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 21107232 | HCID 21107232 | — |
Reaction Steps
A solution of 6-methoxy-4,4,7-trimethyl-3,4-dihydro-2H-naphthalen-1-one (described in U.S. 2003/0166932, published Sep. 4, 2003, incorporated herein by reference; 5.5 g, 25.6 mmol) and sodium cyanide (6.25 g, 127 mmol) in anhydrous dimethylsulfoxide (100 mL) was heated at 230° C. for 48 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 (5.2 g, ˜100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07638648B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-2f612a895aee441980476ac69e8c7179 |
| Source note | uspto-grants-2009_12 |