HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 69686650, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 23391858 | HCID 23391858 | — |
| Catalyst | titanium(III) trichloride | HCID 10313229 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 69686650 | HCID 69686650 | 88.6% |
Reaction Steps
To 100 ml of a solution of 1.85 g of the resulting 3-[(1R,2S)-2-t-butoxycarbonylcyclopropyl]-l-hydroxypyrrolidin-2-one in a 3:1 mixed solvent of methanol and water was added 4.45 ml of a titanium trichloride solution at room temperature while maintaining the reaction mixture neutral by addition of a 1N sodium hydroxide aqueous solution, followed by stirring at the same temperature for 1.5 hours. After completion of the reaction, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give 1.53 g (88.4%) of 3-[(1R,2S)-2-t-butoxycarbonylcyclopropyl]pyrrolidin-2-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06462040B1 |
| Source dataset | uspto-grants-2002_10 |
| ORD ID | ord-b89c812d3581419f89cfb2f080b50a3e |
| Source note | uspto-grants-2002_10 |