HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 87618919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | HCID 87619003 | HCID 87619003 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 87618919 | HCID 87618919 | 74% |
Reaction Steps
A mixture of 50 mL of ethanol, 1 mL of acetic acid and 2.5 g of the (rac)-3-[(5-amino-2-chloro-pyrimidin-4-yl)-(2,2-dimethyl-cyclopentyl)-amino]-propanoic acid ethyl ester (V-59) 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. Trituration of the residue with ether, provided 1.6 g of (rac)-2-chloro-9-(2,2-dimethyl-cyclopentyl)-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VI-59).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07517873B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-38da5e8f0633435da679bb1c7717b14a |
| Source note | uspto-grants-2009_04 |