HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenylacetyl chloride → N-[1-[1,6-Dihydro-6-oxo-1-(phenylmethyl)-3-pyridinyl]cyclohexyl]benzeneacetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenylacetyl chloride | HCID 7679 | — |
| Reactant | 5-(1-aminocyclohexyl)-1-(phenylmethyl)-2(1H)-pyridinone | HCID 9795763 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-[1-[1,6-Dihydro-6-oxo-1-(phenylmethyl)-3-pyridinyl]cyclohexyl]benzeneacetamide | HCID 14989572 | 99.7% |
Reaction Steps
Phenylacetyl chloride (1.6 g) was added to a well stirred suspension of 5-(1-aminocyclohexyl)-1-(phenylmethyl)-2(1H)-pyridinone (2.9 g), poly-4-vinylpyridine (2.1 g) and a catalytic amount of 4-(N,N-dimethylamino)pyridine in 70 ml of dichloromethane, and the resulting mixture was stirred at room temperature for 3 hours. The reaction mixture was filtered and the filtrate concentrated to give 4.1 g of oil. Column chromatography (silica gel, elution with ethyl acetate) afforded 2.1 g of foam. Recrystallization from ethyl acetate/hexanes gave 1.7 g of analytically pure product as needles, m.p. 152°-153° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04978663 |
| Source dataset | uspto-grants-1990_12 |
| ORD ID | ord-821b229471d243d1937fef3d14aab827 |
| Source note | uspto-grants-1990_12 |