HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 17989091, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Isobutyronitrile | HCID 6559 | — |
| Reactant | 2,6-Difluoro-3-methylanisole | HCID 2774135 | — |
| Reactant | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 17989091 | HCID 17989091 | 54.4% |
Reaction Steps
14.48 g (91.56 mmol) of 2,6-difluoro-3-methylanisole is dissolved in 800 ml of toluene. After 272.2 ml (137.35 mmol) of a 0.5 molar solution of potassium hexamethyl disilazide in toluene is added, 25.31 g (366.26 mmol) of isobutyronitrile is added in drops. The batch is stirred for 10 days at room temperature and then added to a 1 M HCl solution. After being extracted three times with methyl-tert-butyl ether, the combined organic extracts are washed with saturated NaCl solution and dried. After spinning-in and chromatography on silica gel (mobile solvent ethyl acetate/hexane), 10.32 g (49.5%) of the desired compound is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08097627B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-dcb39773c03e4698af00800ec5e6f5c1 |
| Source note | uspto-grants-2012_01 |