HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → Diethyl 5-[[(phenylmethoxy)amino]carbonyl]-1,3-benzenedicarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Benzyloxyamine hydrochloride | HCID 102312 | — |
| Reactant | 3,5-Bis(ethoxycarbonyl)benzoate | HCID 22575049 | — |
| Product | Diethyl 5-[[(phenylmethoxy)amino]carbonyl]-1,3-benzenedicarboxylate | HCID 12017544 | 59% |
Reaction Steps
To a solution of diethyl 1,3,5-benzenetricarboxylate (3.192 g, 20 mol) and O-benzylhydroxyamine hydrochloride (4.789 g, 19 mmol) in 40 mL were added N-methylmorpholine (2.2 mL, 20 mmol) and EDC (3.834 g, 20 mmol) at 0° C., and the mixture was stirred at room temperature for 20 hours. The solvent was removed by evaporator and the residue was dissolved in EtOAc (150 mL). The organic solution was washed with 1 N HCL (150 mL), washed with saturated aqueous NaHCO3 (50 mL), dried over Na2SO4, and concentrated to give white solid. This material was recrystallized from EtOAc to give 4.154 g of white powder (59% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06852750B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-960ef9b7f6a741cfb55e760cfcb8604c |
| Source note | uspto-grants-2005_02 |