HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 16091236, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | 1,3-Dichloro-5-iodobenzene | HCID 76424 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 16091236 | HCID 16091236 | 93.2% |
Reaction Steps
To the mixture of LDA (5 mL, 8.6 mmol) in THF (20 mL) was added compound 1,3-dichloro-5-iodobenzene (2.35 g, 8.6 mmol) under −78° C. Then the mixture was added to the pre-cooled solution of (CH3)2SO4 (12 mL, 10.3 mmol) in THF (10 mL) under −78° C. The solution was concentrated under vacuum. The residue was diluted with EA, washed with 1N HCl, 1N NaOH, brine, dried over Na2SO4, concentrated under vacuum to give the desired product (2.3 g, 93% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853186B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-27421eacd31f4e7c81cf1f2965547142 |
| Source note | uspto-grants-2014_10 |