Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2-Chloro-3,5-dinitropyridine | HCID 75738 | — |
| Reactant | 2-Amino-2-thioxoethyl 2,2-dimethylpropanoate | HCID 2782113 | — |
| Solvent | Sulfolane | HCID 31347 | — |
| Product | HCID 44614678 | HCID 44614678 | 16.7% |
Reaction Steps
A mixture of 6 g (29.48 mmol) of 2-chloro-3,5-dinitropyridine and 7.74 g (44.22 mmol) of 2-amino-2-thioxoethyl pivalate in 50 mL of sulfolane is heated for 2 hours at 105° C. After this time, 150 mL of ethyl acetate are added to the mixture, and the organic phase is washed three times with 200 mL of water and then once with 100 mL of saturated sodium chloride solution. The organic phase is then separated out, dried over sodium sulfate and then concentrated under reduced pressure. The product obtained is purified by chromatography on a column of silica, eluting with a mixture of heptane and ethyl acetate. 1.45 g of a yellow solid are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08604050B2 |
|---|
| Source dataset | uspto-grants-2013_12 |
|---|
| ORD ID | ord-64d1a209e8344fb9bde98addbb16824e |
|---|
| Source note | uspto-grants-2013_12 |
|---|