HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 86646688, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | 3-Methoxy-2,2-dimethylpropanoic acid | HCID 3017506 | — |
| Solvent | Thionyl Chloride | HCID 24386 | — |
| Product | HCID 86646688 | HCID 86646688 | 20% |
Reaction Steps
A solution of 3-methoxy-2,2-dimethyl-propionic acid (1.0 g, 7.6 mmol) in thionyl chloride (5 ml) was heated to 50° C. for 16 hours. The reaction mixture was concentrated to a yellow residue and then dissolved in DCM (15 ml). O,N-Dimethyl-hydroxylamine-hydrogen chloride (886 mg, 9.1 mmol) and powdered K2CO3 (2.2 g, 16 mmol) were added, and the reaction mixture was stirred at room temperature for 16 hours. The reaction mixture was filtered through a filter funnel, and the filtrate was collected and concentrated giving a white semisolid. The crude product was purified by silica gel chromatography using 20-50% EtOAc in hexanes as eluant providing 260 mg (20%) of 3,N-dimethoxy-2,2,N-trimethyl-propionamide as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08008298B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-7def7262a2e44fc1a7c871525ebd1110 |
| Source note | uspto-grants-2011_08 |