HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trifluoroacetic acid → (2-Bromophenyl)(2,4,6-trimethoxybenzyl)sulfane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | 2-Bromobenzenethiol | HCID 80598 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 2,4,6-Trimethoxybenzyl alcohol | HCID 602515 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | (2-Bromophenyl)(2,4,6-trimethoxybenzyl)sulfane | HCID 66870845 | 89% |
Reaktionsschritte
To a solution of 30.8 g (2,4,6-trimethoxyphenyl)methanol (155.4 mmol) and 29.2 g 2-bromobenzenethiol (155.4 mmol) in 150 ml DCM at 0° C. was added dropwise 1.3 eq TFA. The reaction was stirred 15 minutes at room temperature before saturated NaHCO3 was added until neutral. The organic volatiles were removed under reduced pressure and the aqueous residue was extracted with ethyl acetate (3×150 ml). The organic layer was collected, washed with brine and dried over magnesium sulfate, filtered, and concentrated under reduced pressure afforded a yellowish solid. The solid was washed with ethyl acetate to yield 51.3 g white solid (2-bromophenyl)(2,4,6-trimethoxybenzyl)sulfane (13.9 mmol, 89% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07550505B2 |
| Quelldatensatz | uspto-grants-2009_06 |
| ORD ID | ord-399fea0165bb4c1f8fcb279647e96072 |
| Quellennotiz | uspto-grants-2009_06 |