HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 20331700, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 2-Amino-6-bromopyridine | HCID 300809 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 20331700 | HCID 20331700 | — |
Reaction Steps
10.0 g (0.0578 mole) of 2-amino-6-bromopyridine was dissolved in 40 ml dry pyridine and 6.4 ml (0.067 mole) of ethyl chloroformate was added dropwise while the solution was stirred and cooled in an ice-bath to maintain the reaction temperature at 15°-18° C. After 4 hours at room temperature, the reaction mixture was poured into 150 ml of ice water and kept at 0° C overnight. Impure 2-ethoxycarbonylamino-6-bromopyridine was obtained by filtration and subsequently recrystallized from 2:1 methanol-water solution, giving an 88% yield of white solid, m.p.=70.2°-71.0° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04048181 |
| Source dataset | uspto-grants-1977_09 |
| ORD ID | ord-20528cdd3af8408eb186036057792f62 |
| Source note | uspto-grants-1977_09 |