HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 135843668, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Boron Trichloride | HCID 25135 | — |
| Reactant | HCID 20634218 | HCID 20634218 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 135843668 | HCID 135843668 | 72.2% |
Reaction Steps
To a mixture of 3-[3-(3-methoxy-2-thienyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)uracil(0.500 g, 1.14 mmol) and methylene chloride at −5° C. is added boron trichloride (1M in methylene chloride, 2.30 ml, 2.3 mmol) via syringe. The resultant mixture is stirred two hours at −5° C., warmed to room temperature, stirred overnight and poured into cold 10% hydrochloric acid. The mixture is extracted with methylene chloride. The organic layer is washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to an oil. The oil is crystallized in ether to afford the title compound as pale yellow-green crystals (0.350 g, 72.2%) which is characterized by NMR spectral analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06706663B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-03f803fbf3b44d4fba1d97ba2159325f |
| Source note | uspto-grants-2004_03 |