HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 1-Acetyl-2-oxo-1,3-diaza-cyclohexane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2(1H)-Pyrimidinone, tetrahydro- | HCID 74615 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 1-Acetyl-2-oxo-1,3-diaza-cyclohexane | HCID 14678122 | — |
Reaction Steps
The mixture of 10 parts by weight of 1,3-diaza-cyclohexan-2-one, 11.8 parts by weight of acetylchloride, 8.7 parts by weight of pyridine, 50 parts by volume of tetrahydrofurane and 50 parts by volume of chloroform was stirred for 24 hours at room temperature, filtered and washed out with tetrahydrofurane chloroform (1:1). The combined solutions were evaporated to dryness, recrystallized from acetone/ethanol; 50 parts by volume of NaHCO3 -solution were added, and the mixture was extracted 3 times with 50 parts by volume of ethylacetate at a time. The combined organic solutions were dried over MgSO4, evaporated to dryness, and the residue was recrystallized from acetone/petrol-ether.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03975375 |
| Source dataset | uspto-grants-1976_08 |
| ORD ID | ord-78441374ad154fb49a85e8c260704833 |
| Source note | uspto-grants-1976_08 |