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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 338144Generated: October 30, 2026

Ethyl Acetate → HCID 89832319, compound

https://huagongshe.com/reaction/338144

Reaction equation

Participants

RoleNameHCIDCharge
ReactantEthyl AcetateHCID 8857—
Reactant1,1,3,3-TetramethylguanidineHCID 66460—
Reactant2-Chloro-5-fluoropyrimidineHCID 583466—
ReactantHCID 89832293HCID 89832293—
SolventDimethyl SulfoxideHCID 679—
SolventWaterHCID 962—
ProductHCID 89832319HCID 8983231943%

Reaction Conditions

Temperature100 °C

Reaction Steps

N,N,N′,N′-tetramethylguanidine (0.44 mL, 3.5 mmol) is added to a solution of racemic N-[7a-(2-fluorophenyl)-4a,5,6,7-tetrahydro-4H-pyrrolo[3,4-d][1,3]thiazin-2-yl]benzamide (1.0 g, 2.9 mmol) and 5-fluoro-2-chloropyrimidine (0.46 g, 3.5 mmol) in dimethylsulfoxide (10 mL). The reaction is stirred at 100° C. for 2 hours, and cooled to room temperature. To the crude reaction is added ethyl acetate (7.5 ml) and water (2.5 ml), the mixture is passed through diatomaceous earth (10 g), and the solvent removed under reduced pressure. The residue is purified by silica gel chromatography eluting with a gradient of 40% to 60% ethyl acetate in hexanes to give the title compound (560 mg, 43%). ES/MS (m/e): 452 (M+H).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08889856B2
Source datasetuspto-grants-2014_11
ORD IDord-4117dc7abf184c8681fcb5aba07beaf3
Source noteuspto-grants-2014_11