HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 54423244, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2,4-Dichloro-6-fluoro-1,3-benzothiazole | HCID 53440570 | — |
| Reactant | HCID 178418443 | HCID 178418443 | — |
| Catalyst | HCID 178418751 | HCID 178418751 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 54423244 | HCID 54423244 | — |
Reaction Steps
A solution of 0.2 mol of ethyl magnesium bromide in diethyl ether was added to a solution of 22.0 g (0.1 mol) of 2,4-dichloro-6-fluorobenzothiazole and 3.3 g (5 mmol) of dichlorobis(triphenylphosphine)nickel in 0.5 1 of diethyl ether. Stirring was carried out for 2 hours, after which the mixture was poured onto saturated aqueous ammonium chloride solution. The product was extracted with diethyl ether. The combined organic phases were washed with water, dried over magnesium sulfate and finally evaporated down. Purification of the crude product was effected by means of silica gel chromatography (eluent: 8:2 cyclohexane/methyl tert-butyl ether). Yield: 10.3 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05888940 |
| Source dataset | uspto-grants-1999_03 |
| ORD ID | ord-5e948661f41d4c2c87f97919c63db590 |
| Source note | uspto-grants-1999_03 |