Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 71224964 | HCID 71224964 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86676000 | HCID 86676000 | 97% |
Reaction Steps
4 mL of a chloroform solution containing 0.45 g (2 mmol) of 2-t-butoxycarbonyl amino-6-methylpyridine-N-oxide and 0.26 g (2 mmol) of diisopropylethylamine was prepared, and was adjusted to 10° C. 0.29 g (2 mmol) of benzoyl chloride was added dropwise to the solution over 10 minutes at 10° C. After stirring further for 40 minutes at 10° C., 5 mL of water was added thereto, followed by liquid separation. The chloroform layer obtained by liquid separation was washed twice with 5 mL of water, and then dried with magnesium sulfate, followed by filtration. The resulting solution was concentrated under reduced pressure and dried to obtain 0.64 g of 2-t-butoxycarbonyl-2-benzoyl amino-6-methylpyridine-N-oxide (yield: 97%) in the form of yellow-brown amorphous which was the target product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08981107B2 |
|---|
| Source dataset | uspto-grants-2015_03 |
|---|
| ORD ID | ord-158056dd50204937a07c10ba66b5e075 |
|---|
| Source note | uspto-grants-2015_03 |
|---|