反应详情

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.

1. stirringthe mixture was stirred for 30 minutes
2. concentrationThe reaction solution was concentrated in vacuo
3. customto give a residue
4. customThe resulting precipitates
5. filtrationwere filtered off
6. concentrationthe filtrate was concentrated
7. distillationThe residue was distilled