HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 86672817, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 67282310 | HCID 67282310 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86672817 | HCID 86672817 | — |
Reaction Steps
Thionyl chloride (0.48 mL, 6.6 mmol) was added dropwise to a suspension of 3-hydroxy-2-(hydroxymethyl)-1-methyl-6-(2,2,2-trifluoro-1-hydroxyethyl)pyridin-4(1H)-one (1.50 g, 5.9 mmol) in acetonitrile (45 mL). The progress of the reaction was monitored by TLC (eluant: methanol:dichloromethane, 15:100, v:v), and the starting material was consumed within 5 min. The reaction mixture was concentrated repeatedly in acetonitrile to give a solid, which was then washed with acetonitrile (15 mL×1). Thus, 2-(chloromethyl)-3-hydroxy-1-methyl-6-(2,2,2-trifluoro-1-hydroxyethyl)pyridin-4(1H)-one hydrochloride was obtained as a white solid (1.18 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073865B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-7b60e897e01d436397d418e767c80945 |
| Source note | uspto-grants-2015_07 |