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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 399556Generated: October 29, 2026

p-Toluenesulfonic acid → HCID 21830556, compound

https://huagongshe.com/reaction/399556

Reaction equation

Participants

RoleNameHCIDCharge
Reactantp-Toluenesulfonic acidHCID 6101—
Reactant3-Chloro-4-fluoroanilineHCID 9708—
ReactantHexamethyldisilazaneHCID 13838—
Reactant6-methylsulfanyl-1H-pyrimido[5,4-d]pyrimidin-4-oneHCID 178503402—
SolventMethanolHCID 887—
ProductHCID 21830556HCID 21830556—

Reaction Conditions

Temperature100 °C

Reaction Steps

148 g of 4-hydroxy-6-methylthiopyrimido[5,4-d]pyrimidine, 286 ml of hexamethyldisilazane, 333 g of 3-chloro-4-fluoroaniline and 15 g of p-toluenesulphonic acid are heated at 140° C. for 23 hours. The reaction mixture is cooled and, after addition of 4 l of methanol, heated at 100° C. for one hour. The methanol is distilled off and the residue is triturated three times with diethyl ether and filtered off with suction.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05821240
Source datasetuspto-grants-1998_10
ORD IDord-b9799cd62b1d419facb50bfff3e3cc1a
Source noteuspto-grants-1998_10