HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-Methylbenzylamine → N-methyl-1-phenyl-N-[(2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran-2-yl)methyl]methanamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-Methylbenzylamine | HCID 7669 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Dimethylacetamide | HCID 31374 | — |
| Reactant | 2-(Iodomethyl)-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran | HCID 15268305 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | N-methyl-1-phenyl-N-[(2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran-2-yl)methyl]methanamine | HCID 66760229 | 75% |
Reaction Steps
N-methylbenzylamine (766 mg, 3.16 mmol) and potassium carbonate (1.09 g, 7.90 mmol) were added to a solution of DMA (5 mL) containing 2-(iodomethyl)-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran (1.00 g, 3.16 mmol) synthesized in Reference Example 126, and the mixture was stirred under heated reflux for 4 hours. The reaction solution was cooled to room temperature, and water and ethyl acetate were added thereto to separate an organic layer. The organic layer was washed with water and saturated saline, and dried using anhydrous magnesium sulfate, followed by concentration under reduced pressure. The residue was purified by silica gel chromatography (hexane-ethyl acetate 99:1-93:7) to give 730 mg of the title compound (yield: 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288390B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-8c4d5d476906495d815bd295bbc14b3b |
| Source note | uspto-grants-2012_10 |