HuagongsheHuagongshe Chemistry Print Report · For research reference only
ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride → ethyl-N-(6-amino-2,3-dichlorobenzyl)glycine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride | HCID 66640009 | — |
| Catalyst | Platinum | HCID 23939 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | ethyl-N-(6-amino-2,3-dichlorobenzyl)glycine | HCID 67080112 | 72% |
Reaction Steps
A solution of 0.344 g of ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride (compound VI) in 1.5 mL of water and 1.5 mL ethanol (with 5% isopropanol) was stirred and 5% sulfided platinum on carbon under hydrogen (50 to 100 psi) for 16 hours. The catalyst was removed by filtration. The filtrate concentrated, diluted with water and toluene, and basified (aqueous sodium hydroxide or potassium carbonate) to pH 9-10. The organic phase was separated, concentrated, and the crude material purified by low-temperature recrystallization from toluene in hexane to give compound I in 72% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06653500B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-5ecaf55e573e49b5b990f95c786a5cfc |
| Source note | uspto-grants-2003_11 |