HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-Dichloro-2-isothiocyanatobenzene → HCID 86664891, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-Dichloro-2-isothiocyanatobenzene | HCID 123239 | — |
| Reactant | HCID 67356496 | HCID 67356496 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86664891 | HCID 86664891 | — |
Reaction Steps
5-Bromo-6-methoxy-N-methyl-3-nitropyridin-2-amine (0.5 g, 1.9 mmol) in THF was combined with Raney nickel (70 mg) and hydrogenated in a Parr apparatus at ambient temperature for 10 h at 3.5 bar hydrogen pressure. Then the mixture was directly filtered into a mixture of 1,3-dichloro-2-isothiocyanatobenzene (0.39 g, 1.9 mmol) in THF and stirred overnight at ambient temperature. The solvent was removed i. vac. and the residue was purified by HPLC (C18 Symmetry, 8 μm, eluent: H2O+0.15% HCOOH+15-100% acetonitrile).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08703796B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-7a8320af200b4c44929c383761698a0d |
| Source note | uspto-grants-2014_04 |