HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 21867201, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Iodobenzylamine hydrochloride | HCID 2723861 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21867201 | HCID 21867201 | — |
Reaction Steps
3-Iodobenzylamine hydrochloride (1.0 g) and diisopropylethylamine (1.29 ml) were taken up in dry dimethylsulfoxide (60 ml) and treated with ethyl bromoacetate and stirred under nitrogen for 2 h. 2M HCl (1.85 ml) and water (250 ml) were added. This was extracted with EtOAc, the aqueous phase was taken to pH 8 and extracted with EtOAc. The combined extracts were dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by chromatography (Biotage, 40 g) eluting with EtOAc-cyclohexane-diisopropylethylamine (10:89:1 then 20:79:1) to give the title compound (0.571 g) LCMS RT 2.02 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07144908B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-e713a09a906548ae9276e057a58685f4 |
| Source note | uspto-grants-2006_12 |