HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22314484, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22314487 | HCID 22314487 | — |
| Product | HCID 22314484 | HCID 22314484 | 53% |
Reaction Steps
A suspension of 2-fluoro-4-(3-fluoro-benzyloxy)-benzonitrile (24.5 g, 100 mmol) and sodium hydroxide (30 g, 750 mmol) in water (300 mL) was heated under reflux for 16 h. After cooling to room temperature the suspension was acidified to pH 2 with concentrated hydrochloric acid. The resulting mixture was diluted with water (100 mL) and extracted with ether (3×400 mL). The combined organic extracts were then washed with water and brine and then dried over sodium sulfate. Filtration and half evaporation of the filtrate resulted in the formation of a white precipitate which was filtered off to afford the title compound (14 g, 53%) as white crystals after recrystallisation from cyclohexane: ethyl acetate. MS: m/e=263.1 (M−H−)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06951884B2 |
| Source dataset | uspto-grants-2005_10 |
| ORD ID | ord-ba53fd82a31a48f7822ebe862dd8aed1 |
| Source note | uspto-grants-2005_10 |