HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoyl isothiocyanate → HCID 86724267, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoyl isothiocyanate | HCID 68284 | — |
| Reactant | HCID 86724268 | HCID 86724268 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 86724267 | HCID 86724267 | 21.3% |
Reaction Steps
Under ice cooling, to a solution of 2-(4-amino-6-bromo-4H-spiro[chromene-3,1′-cyclopropan]-4-yl)-2,2-difluoroethanol (2.24 g, 6.46 mmol) in acetone (45 mL) was added benzoyl isothiocyanate (1.16 g, 7.10 mmol), and the mixture was stirred for 2 hours at room temperature and stirred for 13 hours at 40° C. After concentration, the residue was purified by silica gel chromatography (EtOAc/hexane=1:99-30:70) followed by purification using silica gel chromatography (NH-silicagel, EtOH/CHCl3=0:100-10:90) to give N-{[6-bromo-4-(1,1-difluoro-2-hydroxyethyl)-4H-spiro[chromene-3,1′-cyclopropan]-4-yl]carbamothioyl}benzamide (684 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975415B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-3cf868c3168c47ba963094342fe65908 |
| Source note | uspto-grants-2015_03 |