HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-2-methyl-1H-indene → 4-(3',5'-Di-t-butylphenyl)-2-methylindene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-2-methyl-1H-indene | HCID 12010742 | — |
| Reactant | HCID 178441125 | HCID 178441125 | — |
| Catalyst | HCID 178418751 | HCID 178418751 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 4-(3',5'-Di-t-butylphenyl)-2-methylindene | HCID 12010743 | — |
Reaction Steps
4-Chloro-2-methylindene (6.1 g, 37 mmol) and NiCl2(PPh3)2 (1.8 g, 2.8 mmol) were dissolved in 150 mL of Et2O. 3,5-Di-t-butylphenylmagnesium bromide (10 g, 37 mmol) as a Et2O solution was added to the solution and the reaction was stirred overnight at room temperature. After overnight stirring, the reaction was slowly quenched with H2O to neutralize unreacted Grignard. The solution was subsequently treated with 100 mL of 10% HCl(aq), neutralized with saturated sodium bicarbonate aqueous solution. The organic layer was dried with magnesium sulfate and the solvent was removed by rotary evaporation. The remaining residue was loaded onto a silica gel column and eluted with hexane. Yield was 4.6 g (40%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376409B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-7dbc63b983324b8da8d1d03478b065e9 |
| Source note | uspto-grants-2002_04 |