HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methyl-2,3,4,5,6,7-hexahydro-1H-inden-1-one → 1,3-dimethyl-4,5,6,7-tetrahydro-1H-indene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methyl-2,3,4,5,6,7-hexahydro-1H-inden-1-one | HCID 11105531 | — |
| Reactant | HCID 178418348 | HCID 178418348 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 1,3-dimethyl-4,5,6,7-tetrahydro-1H-indene | HCID 12980169 | 45.7% |
Reaction Steps
Methyl lithium (96 mL, 1.5M, 0.144 mol) was added dropwise to a solution of 4,5,6,7-tetrahydro-1-methyl-indan-3-one (17.7 g, 0.118 mol) in 50 mL of diethyl ether under an argon atmosphere whereupon the reaction mixture was refluxed for 18 hours. The mixture was hydrolyzed, and extracted with diethyl ether. The ether extracts were dried over anhydrous MgSO4 and filtered. To the ether solution 0.5 mL of 6M HCl was added and the solution was stirred for one hour. After this time period the ether solution was washed with water, dried over anhydrous MgSO4, filtered, and concentrated. Distillation at reduced pressure afforded 8.0 g (45 percent) of product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05624878 |
| Source dataset | uspto-grants-1997_04 |
| ORD ID | ord-45d121d831734b0783ea716e112a8f1a |
| Source note | uspto-grants-1997_04 |