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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2386707Generated: November 1, 2026

Water → HCID 66697308, compound

https://huagongshe.com/reaction/2386707

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantCesium carbonateHCID 10796—
Reactant3,4-DifluorobenzonitrileHCID 587203—
Reactant6-[2-(2-Chloro-5-hydroxy-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-4-methyl-4H-benzo[1,4]oxazin-3-oneHCID 66697195—
SolventDimethylacetamideHCID 31374—
ProductHCID 66697308HCID 6669730882.3%

Reaction Steps

To a solution of 6-[2-(2-chloro-5-hydroxy-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-4-methyl-4H-benzo[1,4]oxazin-3-one (Example 1, step 4, 100 mg) in N,N-dimethylacetamide (1.8 ml) were added 3,4-difluorobenzonitrile (41 mg) and cesium carbonate (235 mg). The mixture was heated under microwave conditions for 30 min to 120° C. After cooling to room temperature, water was added and the mixture was extracted with EtOAc. The organic phase was dried (MgSO4), filtered and concentrated to dryness. The product was purified by chromatography (SiO2, cyclohexane/EtOAc 1:0=>1:1) to give 4-{4-chloro-3-[1-methyl-2-(4-methyl-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl)-2-oxo-ethyl]-phenoxy}-3-fluoro-benzonitrile (92 mg). In analogy to Example 1, step 3, this compound was reacted with trifluoromethyl trimethylsilane and tetramethylammonium fluoride to give the title compound (89 mg) as a colorless solid. MS (m/e)=535.1 [M+H+].

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08268820B2
Source datasetuspto-grants-2012_09
ORD IDord-3454bda00c484fcfa48041a6ceb36ce9
Source noteuspto-grants-2012_09