HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 19423622, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 67626345 | HCID 67626345 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19423622 | HCID 19423622 | 96% |
Reaction Steps
To a solution of 480 mg (1 mmol) of 3-[1-(3-methylthiobenzyl)piperidin-4-yl]-4-phenyl-3,4-dihydro -2(1H)-quinazolinone HCl salt in 10 mL of methylene chloride was added 190 mg (1.1 mmol) of m-chloroperbenzoic acid at temperature of 0° C. to 10° C. The mixture was stirred for 10 hours at ambient temperature, mixed with water, adjusted to pH 10 with a aqueous ammonia and then extracted with chloroform. The organic layer separated was washed with brine, dried on sodium sulfate and then concentrated in vacuo. The residue was purified by means of column chromatography (silica gel, 1:9 methanol:chloroform) to give 440 mg (0.96 mmol) of the title compound as an about 1:1 mixture of the diastereomers.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05556860 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-f2fee59fe3f243a0807af8cb574b5ebc |
| Source note | uspto-grants-1996_09 |