HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-[4-(4-Chloro-butyryl)-phenyl]-2-methyl-propionitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tin tetrachloride | HCID 24287 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | 1-Butanone, 1-[4-(1-bromo-1-methylethyl)phenyl]-4-chloro- | HCID 10063579 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-[4-(4-Chloro-butyryl)-phenyl]-2-methyl-propionitrile | HCID 15512830 | — |
Reaction Steps
Dissolve 1-[4-(1-bromo-1-methyl-ethyl)-phenyl]-4-chloro-butan-1-one (2.00 g, 6.59 mmol) in anhydrous methylene chloride (20 mL) and place under an argon atmosphere. Add trimethylsilyl cyanide (1.10 mL, 8.25 mmol) followed by tin (IV) chloride (0.20 mL, 1.7 mmol) via syringe. Stir at reflux for 1 hour, add water (20 mL) and stir for an additional ½ hour. Separate the layers and extract the aqueous layer with methylene chloride. Combine the organic layers, wash with brine, dry (MgSO4), filter and evaporate the solvent in vacuo. Purify by silica gel chromatography (15% ethyl acetate/hexane) to give the title compound as a white solid; mp 79-80° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06340761B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-b2fb9780006a4303b01edf210f805658 |
| Source note | uspto-grants-2002_01 |