HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57925845, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1003315-34-1 | HCID 87354258 | — |
| Reactant | HCID 91145363 | HCID 91145363 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 57925845 | HCID 57925845 | — |
Reaction Steps
2-(Dimethylphosphoryl)ethanamine hydrochloride (393 mg, 2.493 mmol), tert-butyl (3-{[4-(bromomethyl)benzoyl]amino}biphenyl-4-yl)carbamate (400 mg, 0.831 mmol), and DIEA (581 μl, 3.32 mmol) were combined in DMF (8 mL) and water (0.50 mL) and stirred at 60° C. overnight. The solution was diluted with saturated NaHCO3 and extracted with EtOAc (4×). The combined organics were dried (MgSO4), evaporated, and purified by reverse phase HPLC (25-95% MeCN/water w/0.025% TFA). Product fractions were neutralized with saturated NaHCO3, extracted with EtOAc (2×), dried (MgSO4), and evaporated to give a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981874B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-0523f184d3714da588234b2ca9f36b31 |
| Source note | uspto-grants-2011_07 |