HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzaldehyde → (3R,7aS)-3-Phenyltetrahydro-3H,5H-pyrrolo[1,2-c][1,3]oxazol-5-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzaldehyde | HCID 240 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | (S)-5-(Hydroxymethyl)-2-pyrrolidinone | HCID 643511 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | (3R,7aS)-3-Phenyltetrahydro-3H,5H-pyrrolo[1,2-c][1,3]oxazol-5-one | HCID 395160 | — |
Reaction Steps
A suspension of 148.5 g of (S)-5-hydroxymethyl-pyrrolidin-2-one in 891 mL of toluene is treated with 172.1 mL of benzaldehyde at room temperature. p-Toluenesulphonic acid (2.94 g) is added and the reaction mixture stirred at reflux for 20 hours with azeotropic removal of water. The reaction mixture is treated with 500 mL of a 5% solution of sodium hydrogen carbonate in water. The organic layer is separated and washed once with 500 mL of a 40% solution of sodium bisulphite solution followed by 2×250 mL of water. The organic layer is dried with sodium sulphate, filtered and the solvent removed to give an oil. Fractional distillation in vacuum produces pure (3R,7aS)-3-phenyl-tetrahydro-pyrrolo[1,2-c]oxazol-5-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07910774B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-65e9f74607104a698809b522f8ab2457 |
| Source note | uspto-grants-2011_03 |