HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59771240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-(4-Aminophenyl)propane-1,3-diol | HCID 19593976 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 59771240 | HCID 59771240 | 47% |
Reaction Steps
A mixture of 2-(4-amino-phenyl)-propane-1,3-diol (1.6 g, 9.6 mmol, J. Med. Chem., 40(25), 4030-4052, (1997)), di-tert-butyl dicarbonate (BOC)2O (2.30 g, 10.5 mmol), THF (200 mL), water (100 mL) and Na2CO3 (1.12 g, 10.5 mmol) was stirred at RT overnight. The reaction mixture was diluted with EtOAc (200 mL) and satd brine (200 mL). The organic layer was separated and the aq layer was extracted with EtOAc (2×100 mL). The organic layers were combined, dried (Na2SO4) and concentrated. The residue obtained was purified on silica (20-100% EtOAc-hexane) to obtain the title compound (1.2 g, 47%): Mass spectrum (ESI, m/z): Calcd. for C14H21NO4, 290.3 (M+Na). found 290.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973035B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-c9a29bd407ac47c5ae5837515d9d9a92 |
| Source note | uspto-grants-2011_07 |