HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 59900484, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyl 2-[3,5-dichloro-2-methyl-6-oxo-1(6H)-pyrazinyl]acetate | HCID 10663926 | — |
| Reactant | HCID 59900574 | HCID 59900574 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Ammonia | HCID 222 | — |
| Product | HCID 59900484 | HCID 59900484 | 159.4% |
Reaction Steps
Benzyl 2-[3,5-dichloro-2-methyl-6-oxo-1(6H)-pyrazinyl]acetate (preparation 17) (404 mg, 1.23 mmol) was added to a solution of [(2R)-1-cyclopentylpyrrolidinyl]methylamine (preparation 143) (208 mg, 1.23 mmol) in ethyl acetate (10 ml), followed by triethylamine (190 ml, 1.36 mmol), and the reaction heated under reflux overnight under a nitrogen atmosphere. The cooled mixture was diluted with ethyl acetate, washed with water, brine, then dried over MgSO4 and concentrated under reduced pressure. The crude product was purified by chromatography using a Biotage™ (KP-Sil™ 60 Å silica gel) cartridge and an elution gradient of dichloromethane:methanol:0.88 ammonia (100:0:0 to 95:5:0.5) to give the desired product as a cream solid, (450 mg, 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06180627B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-8e2a642100f44c69a93f7edc215c2755 |
| Source note | uspto-grants-2001_01 |