HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68646048, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Nitromethane | HCID 6375 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 87528820 | HCID 87528820 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 68646048 | HCID 68646048 | — |
Reaction Steps
MeNO2 (1.3 mL, 25 mmol) was added dropwise to a stirred solution of crude 4-[2-(5,5-dimethyl-[1,3,2]dioxaborinan-2-yl)-3-formyl-phenoxy]-butyric acid methyl ester (9.4 g), NaOH (1.0 g, 25 mmol) and H2O (35 mL) in MeCN (90 mL) at rt. The mixture was stirred at rt O/N and then acidified (pH 2) using 4 M HCl. The THF was removed in vacuo and the aqueous layer was extracted with EtOAc. The organic layer was washed with brine, dried (MgSO4), and concentrated in vacuo. The residue was purified by flash chromatography (10% to 30% EtOAc in hexane) to give the title compound as a yellow oil: yield 2.52 g (45% over 2 steps).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08895534B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-977711d46dc04f47bf44489ddede8c43 |
| Source note | uspto-grants-2014_11 |