HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → (R)-2-benzyloxycarbonylamino-2-ethoxycarbonylsuccinimide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | (R)-diethyl 2-benzyloxycarbonylamino-2-carbamoylsuccinate | HCID 66725151 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | (R)-2-benzyloxycarbonylamino-2-ethoxycarbonylsuccinimide | HCID 9944916 | 85.2% |
Reaction Steps
A solution of (R)-diethyl 2-benzyloxycarbonylamino-2-carbamoylsuccinate (200 mg) in dehydrated ethanol (10 mL) was added with sodium ethoxide (41 mg) with ice cooling and stirring, the mixture was stirred at the same temperature for 2 hours, then cold 1 mol/L hydrochloric acid was poured into the mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was recrystallized from ethyl acetate/n-hexane to obtain the title compound (149 mg, yield: 85%) as colorless crystals. Optical rotation [α]D28 was −31.8° (c 0.59, ethanol), and optical purity was 99.2% ee.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434737B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-98f5a7135b264582b0e00a905088e780 |
| Source note | uspto-grants-2016_09 |