HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Naphthoic acid → N-(2-(methoxy(methyl)amino)-2-oxoethyl)-2-naphthamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Naphthoic acid | HCID 7123 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-amino-N-methoxy-N-methylacetamide | HCID 10329278 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(2-(methoxy(methyl)amino)-2-oxoethyl)-2-naphthamide | HCID 45866900 | — |
Reaction Steps
To a mixture of 2-naphthoic acid (5.8 g, 33.7 mmol), 2-amino-N-methoxy-N-methylacetamide (Gly Weinreb amide; prepared from Boc-Gly Weinreb amide 15 as in Example 44) (3.8 g, 32.1 mmol) and DIPEA (12.0 mL, 68.9 mmol) in DCM (70 mL) was added BOP (14.9 g, 33.7 mmol) in one portion at room temperature. The resulting mixture was stirred for 1 hr then saturated NaHCO3 aqueous solution was added. The organic layer was washed with brine (5×60 mL) and 1 N HCl (2×30 mL), dried over MgSO4, filtered and concentrated under reduced pressure to give the crude product, which was used in the next reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08343958B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-5217750aff5145eab329af0ccadb436f |
| Source note | uspto-grants-2013_01 |