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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2257748Generated: October 25, 2026

Water → HCID 22923376, compound

https://huagongshe.com/reaction/2257748

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
Reactant3-[1-(4-Chloro-6,7-dimethoxy-1-phthalazinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1,6-dimethyl-2,4-dioxo-quinazolineHCID 22923461—
CatalystPalladiumHCID 23938—
SolventAcetic AcidHCID 176—
ProductHCID 22923376HCID 2292337619%

Reaction Conditions

Temperature40 °C

Reaction Steps

In 10 ml of acetic acid was dissolved 300 mg (0.61 mmol) of Compound 76 obtained in Example 58, and 40 mg of 10% palladium on carbon suspended in a small amount of water was added to the solution, followed by vigorous stirring at 40° C. for 3 hours under a hydrogen atmosphere at atmospheric pressure. The reaction mixture was filtered using a filter aid, and the filtrate was neutralized by addition of a saturated aqueous solution of sodium bicarbonate and extracted with ethyl acetate. The organic layer was washed successively with water and a saturated aqueous solution of sodium chloride, and then dried. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: chloroform/methanol=50/1). Ether was added to the product, and the precipitated crystals were collected by filtration, washed, and dried to give 52.9 mg (yield: 19%) of Compound 77 as white crystals.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05658917
Source datasetuspto-grants-1997_08
ORD IDord-ade344ac390e46d9900564a58f592390
Source noteuspto-grants-1997_08