HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → HCID 23155961, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | HCID 23155901 | HCID 23155901 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 23155961 | HCID 23155961 | 78% |
Reaction Steps
To a mixed solution of 29 ml of acetone and 1 ml of water, 229 mg of 3-amino-6,6-ethylenedioxy-2-[4-(4-quinolin-2-ylpiperazin-1-yl)butyl]-5,6,7,8-tetrahydro-3H-quinazolin-4-one as synthesized in Example 4-66 and 59 mg of pyridinium p-toluenesulfonate were added and heated under reflux for 112 hours. After cooling, the reaction mixture was extracted with methylene chloride, washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Purifying the residue on silica gel column chromatography (methanol:methylene chloride=1:9) to provide 194 mg (78%) of 6,6-ethylenedioxy-3-isopropylideneamino-2-[4-(4-quinolin-2-ylpiperazin-1-yl)butyl]-5,6,7,8-tetrahydro-3H-quinazolin-4-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07799775B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-9ca7afcfa35c4081a7cf46843fa69ec1 |
| Source note | uspto-grants-2010_09 |