HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 3-(3-(4-Phenoxymethyl-benzyl)-isoxazol-5-yl)-pyridin-2,6-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Ethynylpyridine-2,6-diamine | HCID 55281676 | — |
| Reactant | (4-Phenoxymethyl-phenyl)-acetohydroximoyl chloride | HCID 72262854 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-(3-(4-Phenoxymethyl-benzyl)-isoxazol-5-yl)-pyridin-2,6-diamine | HCID 59255107 | 34.7% |
Reaction Steps
To a tetrahydrofuran (3 mL) solution of (4-phenoxymethyl-phenyl)-acetohydroximoyl chloride (150 mg, 0.545 mmol) described in Manufacturing Example 86-1-5 and 3-ethynyl-pyridin-2,6-diamine (46.3 mg, 0.348 mmol) described in Manufacturing Example 13-1-3 was added triethylamine (104 μL, 0.747 mmol), which was stirred for 1 hour at room temperature. This mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by NH silica gel column chromatography (ethyl acetate) to obtain the title compound (45 mg, 22%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07691882B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-713b14bf9652455ba38f0d53e4a327ab |
| Source note | uspto-grants-2010_04 |