HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylcarbamoyl Chloride → tert-Butyl 6-cyano-2-pyridylmethylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | tert-Butyl 2-pyridylmethylcarbamate N-oxide | HCID 86596464 | — |
| Solvent | Nitroethane | HCID 6587 | — |
| Product | tert-Butyl 6-cyano-2-pyridylmethylcarbamate | HCID 22939432 | 58% |
Reaction Steps
tert-Butyl 2-pyridylmethylcarbamate N-oxide (3.0 g, 13.3 mmol) was dissolved in nitroethane (50 ml), and trimethylsilyl cyanide (2.8 g, 28.6 mmol) and N,N-dimethylcarbamoyl chloride (1.7 g, 16.2 mmol) were added thereto. The mixture was stirred at room temperature for 24 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with ethyl acetate-hexane (2:1, v/v) were collected, concentrated and recrystallized from hexane-ethyl acetate to give the titled compound (1.8 g, 58%) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07399759B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-13c3cde350b843aeb5a8b8ba42d925ab |
| Source note | uspto-grants-2008_07 |