HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbamate → HCID 22669293, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbamate | HCID 276 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Acetic acid, 2-(4-formylphenoxy)- | HCID 89177 | — |
| Reactant | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Product | HCID 22669293 | HCID 22669293 | — |
Reaction Steps
The crude carbamate (0.257 g, 0.84 mmol) was deprotected by stirring in 4N HCl—dioxane (15 mL) for 2 h at room temperature. Volatiles were removed under reduced pressure to give a pinkish solid. 4-Formylphenoxyacetic acid (0.200 g, 1.1 mmol) was dissolved in DCM (3 mL) and DIEA (0.5 mL) was added followed by TBTU (0.350 g, 1,1 mmol) and the amine salt from above (0.240 g, 1 mmol). The mixture was stirred 4 h at room temperature, dissolved in EtOAc and washed sequentially with 5% aqueous K2CO3, KHSO4, water and brine. The extract was dried (MgSO4) and concentrated under reduced pressure to give an off-white solid (0.162 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07439258B2 |
| Source dataset | uspto-grants-2008_10 |
| ORD ID | ord-0c14e45ea2ed416b9b0bdded8b4b7d95 |
| Source note | uspto-grants-2008_10 |