HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dibromomethane → 4-Methyl-[1,3]dioxolo[4,5-c]pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dibromomethane | HCID 3024 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Methyl-3-hydroxy-4-pyridone | HCID 66605815 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | 4-Methyl-[1,3]dioxolo[4,5-c]pyridine | HCID 19926451 | — |
Reaction Steps
2-Methyl-3-hydroxy-4-pyridone (1.25 g, 10 mmol) was dissolved in dry DMSO (20 ml). Dibromomethane (3.5 g, 20 mmol) was added followed by sodium hydride (1 g, >20 mmol, 50-60% in oil). The mixture was left at ambient temperature under stirring for 3 days whereupon it was poured into brine (50 ml). The water-DMSO solution was extracted with methylene chloride (3×50 ml) and the collected extracts were used directly in the next step. A sample for NMR analysis was withdrawn.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05430042 |
| Source dataset | uspto-grants-1995_07 |
| ORD ID | ord-de054ac5c3074316a6b58a239a592cf6 |
| Source note | uspto-grants-1995_07 |