HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4-Dichloro-1-isothiocyanatobenzene → HCID 86632864, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4-Dichloro-1-isothiocyanatobenzene | HCID 81066 | — |
| Reactant | HCID 68737549 | HCID 68737549 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86632864 | HCID 86632864 | 56% |
Reaction Steps
To a solution of ethyl N-(2,6-diaminophenyl)-beta-alaninate (Reference Example 25; 500 mg, 2.24 mmol) in tetrahydrofuran (22 mL) was added 2,4-dichlorophenyl isothiocyanate (503 mg, 2.46 mmol) at room temperature. The resultant mixture was stirred at room temperature for 1 hr and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel eluting with a 10-40% ethyl acetate/n-hexane gradient mixture and NH-silica gel eluting with a 10-90% ethyl acetate/n-hexane gradient mixture to give the title compound as a solid (533 mg, 1.25 mmol, 56%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901141B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-b1147e2219d04508834dd02f59e38aeb |
| Source note | uspto-grants-2014_12 |