HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-(1-Cyanocyclopropyl)benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,2-Dibromoethane | HCID 7839 | — |
| Reactant | 4-(Cyanomethyl)benzoic acid | HCID 270871 | — |
| Catalyst | Benzyl triethylammonium chloride | HCID 66133 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | 4-(1-Cyanocyclopropyl)benzoic acid | HCID 59556707 | — |
Reaction Steps
To 2 g (12.4 mmol) of 4-(cyanomethyl)benzoic acid (Ubichem, Eastleigh, UK) and 10.9 ml (124 mmol) 1,2-dibromoethane (Fluka, Buchs, Switzerland) cooled at 0° C. with an ice-bath are added a solution of 14.4 g (62 mmol) benzyltriethylammonium chloride in 50 ml 8 M aqueous NaOH. The reaction mixture is stirred over night at rt and then is acidified at pH 1-2 with 6 M aqueous HCl and is extracted with EtOAc. The organic layer is washed with H2O (2×) and evaporated to dryness. The solid is triturated in MeOH to provide the crude title compound. ES-MS: 186 (M−H)−; analytical HPLC: tret=4.43 minutes (Grad 2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08431592B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-4e3304f3832444b2b61eb9635277ce1a |
| Source note | uspto-grants-2013_04 |