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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2203055Generated: November 1, 2026

Tributylphosphine → HCID 89691345, compound

https://huagongshe.com/reaction/2203055

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTributylphosphineHCID 13831—
Reactant1,1'-(Azodicarbonyl)dipiperidineHCID 73042—
Reactant219765-84-1HCID 22388014—
Reactant1-(2-cyclopropyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-oneHCID 89691084—
SolventTetrahydrofuranHCID 8028—
SolventEthyl AcetateHCID 8857—
ProductHCID 89691345HCID 8969134525.1%

Reaction Conditions

Temperature60 °C

Reaction Steps

To a mixture of 1-(2-cyclopropyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one (100 mg), (2,5-dichloro-3-thienyl)methanol (130 mg), tributylphosphine (0.264 ml) and THF (10 ml) was added 1,1′-(azodicarbonyl)dipiperidine (269 mg), and the mixture was stirred at 60° C. for 2 h. The reaction mixture was diluted with EtOAc, washed with water and brine successively, dried over MgSO4, and concentrated in vacuo. The residue was purified by NH silica gel column chromatography (hexane/EtOAc), followed by silica gel column chromatography (hexane/EtOAc then EtOAc/MeOH) to give the title compound (39.9 mg) as an off-white solid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09365540B2
Source datasetuspto-grants-2016_06
ORD IDord-357ebd6923074484b43bae13ec82387c
Source noteuspto-grants-2016_06