HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178486878, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 6-Hydroxy-7-methoxy-3,4-dihydroquinazolin-4-one | HCID 135446413 | — |
| Reactant | HCID 178481023 | HCID 178481023 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 178486878 | HCID 178486878 | 62.6% |
Reaction Steps
2.4 g sodium carbonate are added to 2 g of 3,4-dihydro-4-oxo-6-hydroxy-7-methoxy-quinazoline (VII) in 16 ml N-methyl-2-pyrrolidinone at 130° C. Then six times 600 mg (in total: 2.4 g) (trans)-1-methanesulphonyloxy-4-(4-methyl-3-oxo-piperazin-1-yl)-cyclohexane (II) are added stepwise at 130° C. within 4 h and the mixture is kept at 130° C. for 20 h. After 10 days, 25 ml of water are added and the mixture is extracted with 25 ml isopropyl acetate, 50 ml of dichloromethane and 25 ml of dichloromethane. The organic phases are evaporated down and the residue is separated off by preparative HPLC. 500 mg of the product are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08263768B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-fa352776a7e644e2b2d4e3b2ade124d5 |
| Source note | uspto-grants-2012_09 |