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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 63618Generated: October 26, 2026

Sulfuric Acid → HCID 118598114, compound

https://huagongshe.com/reaction/63618

Reaction equation

Participants

RoleNameHCIDCharge
ReactantSulfuric AcidHCID 1118—
ReactantTrimethylsilyl cyanideHCID 82115—
ReactantAluminum(III) ChlorideHCID 6451240—
Reactant7-bromo-3,4-dihydro-2H-1-benzopyran-4-oneHCID 22335736—
SolventAcetic AcidHCID 176—
SolventWaterHCID 962—
SolventTolueneHCID 1140—
ProductHCID 118598114HCID 11859811445%

Reaction Conditions

Temperature40 °C

Reaction Steps

To a solution of 7-bromochroman-4-one (2.0 g, 8.8 mmol) and AlCl3 (118 mg, 0.9 mmol) in toluene (10 mL) was added TMSCN (1.3 mL, 9.7 mmol). The solution was stirred at 40° C. for 1.5 h. The reaction was cooled to rt, and H2SO4 (1.0 mL) was added, followed by AcOH (13 mL) and more H2SO4 (4.3 mL). The reaction was heated to 130° C. and stirred for 6 h. The reaction was cooled, poured over H2O (100 mL) and filtered. The filter cake dissolved in THF (50 mL) and filtered. The combined organic solutions were concentrated to give 1.0 g (45%) of the crude title compound as an off-white solid. [M+H] calc'd for C10H8BrNO2, 254, 256. found 254, 256.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09447046B2
Source datasetuspto-grants-2016_09
ORD IDord-4c7efe1c71174b10acaa9f517e2027b1
Source noteuspto-grants-2016_09