HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → HCID 58464908, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | N-methyliminodiacetic acid | HCID 20441 | — |
| Reactant | (5-Bromo-2-fluoro-3-methylphenyl)boronic acid | HCID 44558191 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58464908 | HCID 58464908 | 86% |
Reaction Steps
To a 50 mL round bottom flask equipped with a stir bar was added 5-bromo-2-fluoro-3-methylphenylboronic acid (1.0 g, 4.3 mmol), N-methyliminodiacetic acid (0.76 g, 5.2 mmol), toluene (8 mL) and DMSO (2 mL). The flask was fitted with a Dean-Stark trap and the Dean-Stark trap was fitted with a reflux condenser. The mixture was heated to reflux with azeotropic removal of water for 4.5 h. The solution was concentrated in vacuo. The residue was absorbed on Celite in vacuo from an acetone suspension and the resulting powder was subjected to Isco flash chromatography eluted with 0 to 70% acetonitrile in ether to give 2-(5-bromo-2-fluoro-3-methylphenyl)-6-methyl-1,3,6,2-dioxazaborocane-4,8-dione (1.26 g, 86%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436001B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-19b9b466d2bb46d5a70e9588cd2e1ddb |
| Source note | uspto-grants-2013_05 |