HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → HCID 117675688, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 117675686 | HCID 117675686 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 117675688 | HCID 117675688 | 53.8% |
Reaction Steps
To a mixture of tert-butyl (3R)-3-[(5-carbamoyl-6-{[4-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)phenyl]amino}pyrazin-2-yl)amino]pyrrolidine-1-carboxylate (10 g), chloroform (200 mL) was added N-bromosuccinimide (3.46 g) under ice-cooling, followed by stirring for 1 hour. To the reactant was added silica gel, and the solvent was evaporated under reduced pressure and then purified by silica gel column chromatography (eluent; chloroform:methanol:28% aqueous ammonia=1:0:0-400:10:1) to obtain tert-butyl (3R)-3-[(3-bromo-5-carbamoyl-6-{[4-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)phenyl]amino}pyrazin-2-yl)amino]pyrrolidine-1-carboxylate (6.17 g) as a yellow amorphous substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085540B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-be3f6df812fa43a99a1fbe01d7fcbe2a |
| Source note | uspto-grants-2015_07 |