HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 178468685, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Chloromethyl-3,4-dimethoxypyridinium chloride | HCID 16216928 | — |
| Reactant | HCID 178468686 | HCID 178468686 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178468685 | HCID 178468685 | 71% |
Reaction Steps
5-Carbethoxy-2-mercapto-1H-benzimidazole (2.0 g, 9 mmol) and NaOH (0.36 g, 9 mmol) in H2O (1 ml) were dissolved in ethanol (30 ml). 3,4-dimethoxy-2-chloromethylpyridine hydrochloride (≈6.6 mmol) as a crude material were added and the mixture was heated to boiling. NaOH (0.26 g, 6.6 mmol) in H2O (1 ml) was added and the reflux was continued for 6 hours. The solvent was evaporated off and the residue was diluted with methylene chloride and water. The organic phase was dried over Na2SO4 and the solvent removed under reduced pressure. Crystallizing from CH3CN gave the desired product (1.75 g, 71%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05430042 |
| Source dataset | uspto-grants-1995_07 |
| ORD ID | ord-3851d0dba86647408d62d61255778a81 |
| Source note | uspto-grants-1995_07 |