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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 629945Generated: October 30, 2026

Carbonic acid-guanidine (1:1) → HCID 178476979, compound

https://huagongshe.com/reaction/629945

Reaction equation

Participants

RoleNameHCIDCharge
ReactantCarbonic acid-guanidine (1:1)HCID 286947—
Reactant(E)-ethyl 2-(4-(2-(3-(diethoxyphosphoryl)-3,3-difluoropropoxy)ethoxy)-2-methoxybenzylidene)-3-oxobutanoateHCID 86667771—
SolventMethanolHCID 887—
SolventWaterHCID 962—
SolventEthyl AcetateHCID 8857—
ProductHCID 178476979HCID 17847697915%

Reaction Conditions

Temperature80 °C

Reaction Steps

To a solution of (E)-ethyl 2-(4-(2-(3-(diethoxyphosphoryl)-3,3-difluoropropoxy)ethoxy)-2-methoxybenzylidene)-3-oxobutanoate (1 equiv.) in MeOH (0.20 M) was added guanidine carbonate (1.1 equiv.) and the reaction mixture was heated to 80° C. for 3 h. At this point the reaction mixture was allowed to cool to room temperature and it was then diluted with water and EtOAc. The resulting mixture was transferred to a separatory funnel and washed with EtOAc three times. The combined organic layers were dried over anhydrous Na2SO4 and the volatiles were removed in vacuo. The resulting residue was purified by a COMBIFLASH™ system using a gradient of 0-10% MeOH/DCM to provide the title compound (15%) as a solid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09315530B2
Source datasetuspto-grants-2016_04
ORD IDord-9b7b628470c649d480e70beccb29b8ad
Source noteuspto-grants-2016_04