HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 12815959, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4-chloro-N-methylpiperidine | HCID 79342 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Reactant | HCID 12815954 | HCID 12815954 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12815959 | HCID 12815959 | 98.9% |
Reaction Steps
A solution of a Grignard reagent is prepared by a reaction of 12.0 g of 4-chloro-1-methylpiperidine with 2.4 g of magnesium in 70 ml of tetrahydrofuran and is treated dropwise for 10 minutes with a solution of 21.2 g of 2-(2,5-difluorophenylthio)-5(trifluoromethylthio)benzaldehyde in 40 ml of tetrahydrofuran. The mixture is refluxed for 5 hours and, after cooling, decomposed with a 20% ammonium chloride solution and extracted with benzene. The extract is washed with water, dried with potassium carbonate and evaporated. There are obtained 26.9 g of crude oily α-(1-methyl-4-piperidyl)-2-(2,5-difluorophenylthio)-5-(trifluoromethylthio)benzyl alcohol which is used in this state for further reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04431808 |
| Source dataset | uspto-grants-1984_02 |
| ORD ID | ord-79a89058f24d4064a58ceeb67c78c1e2 |
| Source note | uspto-grants-1984_02 |