HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 21409554, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | (2-Hydroxy-3,3-dimethyl-2H-1-benzofuran-5-yl) methanesulfonate | HCID 536079 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21409554 | HCID 21409554 | 97% |
Reaction Steps
A solution of thionyl chloride (72 parts) in methylene chloride (270 parts) was added dropwise over a period of 30 minutes to a mixture of 2,3-dihydro-2-hydroxy-3,3-dimethyl-5-benzofuranyl methanesulphonate (130 parts) and pyridine (48 parts) in methylene chloride (1,300 parts) cooled in an ice bath. After stirring for three hours, the solution was washed twice with water, dried over sodium sulphate and the solvent distilled off under reduced pressure. The brown liquid which remained solidified to form 2-chloro-2,3-dihydro-3,3-dimethyl-5-benzofuranyl methanesulphonate (135 parts, 97% yield), melting point 59°-61° C, confirmed by its elemental analysis:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04001003 |
| Source dataset | uspto-grants-1977_01 |
| ORD ID | ord-1d0aec94337e45ef836564cb3f822755 |
| Source note | uspto-grants-1977_01 |