Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| Reactant | 3,4-Dimethylbenzyl alcohol | HCID 23407 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Pentane | HCID 8003 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12180345 | HCID 12180345 | 22.5% |
Reaction Steps
A solution, cooled to 0° C., of 6.81 g of 3,4-dimethylbenzyl alcohol and 11.62 ml of N,N,N′,N′-tetramethyl-ethylenediamine in 150 ml of pentane was treated with 62.5 ml of n-butyllithium solution (1.6M in hexane). The reaction mixture was boiled at reflux for 11 hrs. Then, 12.69 g of iodine in 50 ml of THF were added dropwise at −30° C. The mixture was stirred for 15 min. at −30° C. and then left to warm to room temperature. The reaction mixture was added to 100 ml of 10% sulphuric acid. The crude product was isolated by extraction and purified by chromatography on silica gel. There were obtained 2.95 g of (2-iodo-4,5-dimethyl-phenyl)-methanol as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06476264B2 |
|---|
| Source dataset | uspto-grants-2002_11 |
|---|
| ORD ID | ord-35525d467f214c5dbe164b5d7bc023a9 |
|---|
| Source note | uspto-grants-2002_11 |
|---|