HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 53871027, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2,4-Dichloro-6-fluoro-1,3-benzothiazole | HCID 53440570 | — |
| Reactant | HCID 178418332 | HCID 178418332 | — |
| Catalyst | HCID 178418751 | HCID 178418751 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 53871027 | HCID 53871027 | 49.6% |
Reaction Steps
67 ml of a solution of methyl magnesium chloride in tetrahydrofuran (3M; 0.2 mol) were added dropwise to a solution of 22 g (0.1 mol) of 2,4-dichloro-6-fluorobenzothiazole and 3.3 g (5 mmol) of dichlorobis(triphenylphosphine)nickel in 100 ml of diethyl ether. After stirring had been carried out for 2 hours, the mixture was poured onto saturated aqueous ammonium chloride solution. The desired product was extracted with diethyl ether, after which the combined organic phases were washed with water, dried over magnesium sulfate and finally evaporated down. 10 g of the desired product were obtained by crystallization from petroleum ether.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05888940 |
| Source dataset | uspto-grants-1999_03 |
| ORD ID | ord-82e7a942b1ef455fb8614a838e5d0e60 |
| Source note | uspto-grants-1999_03 |