HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 87617704, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | HCID 87617669 | HCID 87617669 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 87617704 | HCID 87617704 | 80.6% |
Reaction Steps
A mixture of 50 mL of ethanol, 1 mL of acetic acid and 2.6 g of the (rac)-3-[(5-amino-2-chloro-pyrimidin-4-yl)-(3-methyl-cyclopentyl)-amino]-propanoic acid ethyl ester (V-58) prepared in the previous step was heated at reflux overnight, and then concentrated under reduced pressure. The residue was taken up in dichloromethane and washed successively with 10% sodium bicarbonate solution, and then water and dried over anhydrous sodium sulfate. The mixture was filtered and then concentrated under reduced pressure to the crude product. Trituration of the residue with ether, provided 1.8 g of (rac)-2-chloro-9-(3-methyl-cyclopentyl)-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VI-58).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07517873B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-5ff520f2098f46c6ae92ae57c4922350 |
| Source note | uspto-grants-2009_04 |