HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59408361, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | (3-Bromopropyl)benzene | HCID 12503 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4-(1,4-Dioxa-spiro(4.5)dec-8-yl)-cyclohexanone | HCID 810913 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59408361 | HCID 59408361 | — |
Reaction Steps
A solution of 160 g (0.67 mol) of 4-(1,4-dioxaspiro[4.5]dec-8-yl)cyclohexanone in 600 ml of THF is added to a solution of the Grignard reagent generated from 147 g (0.74 mol) of p-bromopropylbenzene and 18.0 g (0.74 mol) of magnesium turnings (400 ml of THF). When the addition is complete, the mixture is heated under reflux for 1 h, and sat. ammonium chloride soln. is added. The mixture is acidified using dil. hydrochloric acid and extracted a number of times with MTBE. The combined organic phases are washed with water, and the solution is dried using sodium sulfate. The crude product obtained after removal of the solvents is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08273264B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-f9b3531d992c4f89bd19f449c6ba2345 |
| Source note | uspto-grants-2012_09 |