HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitroethane → tert-Butyl 6-cyano-2-pyridylmethylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitroethane | HCID 6587 | — |
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | tert-butyl methyl(2-pyridyl)carbamate N-oxide | HCID 86596460 | — |
| Product | tert-Butyl 6-cyano-2-pyridylmethylcarbamate | HCID 22939432 | 77% |
Reaction Steps
A mixture of tert-butyl methyl(2-pyridyl)carbamate N-oxide (14.1 g, 63 mmol), trimethylsilyl cyanide (12.5 g, 126 mmol), N,N-dimethylcarbamoyl chloride (13.5 g, 125 mmol) and nitroethane (120 ml) was stirred at room temperature for 48 hrs. The reaction mixture was concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography, eluted with hexane-ethyl acetate (10:1, v/v) and recrystallized from ethyl acetate-hexane to give the titled compound (11.3 g, 77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07767665B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-9d10c311de32489ca938bb3545092a02 |
| Source note | uspto-grants-2010_08 |