HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-(1,3-Dioxan-2-yl)-3-fluorobenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,3-Propanediol | HCID 10442 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | 3-Fluoro-4-formylbenzonitrile | HCID 2783150 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-(1,3-Dioxan-2-yl)-3-fluorobenzonitrile | HCID 58032581 | — |
Reaction Steps
4-Cyano-2-fluorobenzaldehyde (65 g, 436 mmol) and 1,3-propanediol (36.5 g, 479 mmol; 1.1 eq.) were, together with 4-toluenesulfonic acid monohydrate (1.66 g, 8.72 mmol; 0.02 eq.), initially charged in toluene (1000 ml) and stirred at boiling point on a water separator for 6 h. The reaction mixture was then washed with saturated sodium bicarbonate solution (3×300 ml) and saturated sodium chloride solution (3×300 ml). The organic phase was dried over sodium sulfate and concentrated. The title compound was obtained as a solid (92 g, quant.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174997B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-24975f5f795c4a6bbff2c740407df9f5 |
| Source note | uspto-grants-2015_11 |