HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-(9-cyclopentyl-5,7,7-trimethyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxybenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2486-69-3 | HCID 288057 | — |
| Reactant | 2-Chloro-9-cyclopentyl-5,7,7-trimethyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one | HCID 59295116 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-(9-cyclopentyl-5,7,7-trimethyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxybenzoic acid | HCID 42610787 | 52% |
Reaction Steps
A mixture of 25.26 g (0.0818 mole) 2-chloro-9-cyclopentyl-5,7,7-trimethyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-38), 15.35 g (0.0900 mole) of 4-amino-3-methoxy-benzoic acid, 300 mL of ethanol and 1200 mL of 1M hydrochloric acid was heated at reflux for 17 hours. The mixture was cooled, and the precipitate which formed was collected by filtration to give 18.7 g of 4-(9-cyclopentyl-5,7,7-trimethyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-benzoic acid (I-38) as white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07517873B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-27a714fe0a8743d69a5e9b1ab5b31c7a |
| Source note | uspto-grants-2009_04 |