HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 10012185, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | Butanoyl chloride, 2-oxo- | HCID 11007880 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10012185 | HCID 10012185 | — |
Reaction Steps
Ethyloxalyl chloride (15.2 g, 92.7 mmol) and N,O-dimethylhydroxylamine hydrochloride (9.00 g, 92.3 mmol) were added to chloroform (180 ml) at 0° C. To the mixture was gradually added triethylamine (18.6 g, 184 mmol) under stirring. After the mixture was allowed to warm up to room temperature, the mixture was stirred for 30 minutes, and then methanol (30 ml) was added thereto. The reaction solution was concentrated in vacuo to give a residue, to which was added tetrahydrofuran. The resulting precipitates were filtered off, and the filtrate was concentrated. The residue was distilled to give the title compound (7.47 g) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06914062B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-3ec27d4a118a4dd3870831533623a72c |
| Source note | uspto-grants-2005_07 |