HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86757174, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 86757173 | HCID 86757173 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86757174 | HCID 86757174 | 88% |
Reaction Steps
Phosphorus tribromide (1 ml, 10.7 mmol) is added drop by drop with a syringe at between 20 and 25° C. to a solution of the previous 6-(hydroxymethyl-4,4-dimethyl-3,4-dihydro-2H-1-benzothiopyrane (1.85 g, 8.9 mmol) in 6.2 ml of anhydrous toluene. The mixture was left to agitate for 1 hour and then hydrolysed at 0° C. by ice and then by water. This was then extracted with ethyl ether, dried over MgSO4, filtered and the solvents evaporated. 2.14 g of 6-(bromomethyl-4,4-dimethyl-3,4-dihydro-2H-1-benzothiopyrane is obtained (gross yield=88%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06265423B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-28434322ef704df0afa2dcd15180acc7 |
| Source note | uspto-grants-2001_07 |