Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1398787Generated: October 31, 2026

Sodium Bicarbonate → HCID 68765177, compound

https://huagongshe.com/reaction/1398787

Reaction equation

Participants

RoleNameHCIDCharge
ReactantSodium BicarbonateHCID 516892—
Reactantp-Toluenesulfonic acid monohydrateHCID 521998—
Reactant2,2-Difluoro-1,3-dioxaindan-4-amineHCID 2736891—
ReactantEthyl 4-[2,4-dichloro-7-(1-ethylpropyl)-1H-benzimidazol-1-yl]butanoateHCID 68761768—
SolventO-XyleneHCID 7237—
ProductHCID 68765177HCID 6876517781%

Reaction Conditions

Temperature150 °C

Reaction Steps

A mixture of ethyl 4-[2,4-dichloro-7-(1-ethylpropyl)-1H-benzimidazol-1-yl]butanoate (Reference Example 33; 815 mg, 2.19 mmol), 4-amino-2,2-difluoro-1,3-benzodioxole (950 mg, 5.49 mmol), p-toluenesulfonic acid monohydrate (416 mg, 2.19 mmol) and xylene (3.0 mL) was stirred at 150° C. for 2 hr. The mixture was neutralized with aqueous sodium hydrogen carbonate and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel eluting with a 0-20% ethyl acetate/n-hexane gradient mixture. The filtrate was concentrated in vacuo to give the solid, which was washed with n-hexane to give the title compound as a colorless powder (900 mg, 1.77 mmol, 81%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08901141B2
Source datasetuspto-grants-2014_12
ORD IDord-59d828cf910b4a22b9bf630aa2521553
Source noteuspto-grants-2014_12