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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2353988Generated: November 2, 2026

Phosphorus oxide (P4O10) → HCID 59003108, compound

https://huagongshe.com/reaction/2353988

Reaction equation

Participants

RoleNameHCIDCharge
ReactantPhosphorus oxide (P4O10)HCID 14812—
ReactantHydrazine hydrate (1:1)HCID 24654—
ReactantHCID 86616088HCID 86616088—
SolventMethanolHCID 887—
SolventWaterHCID 962—
ProductHCID 59003108HCID 59003108—

Reaction Conditions

Temperature70 °C

Reaction Steps

To a mixture of N-(3,5-Bis-trifluoromethyl-benzyl)-N-[8-chloro-1-(3-oxo-butyryl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl]-acetamide (0.13 mmol, 72 mg), hydrazine hydrate (1.3 mmol, 40.0 μL) in MeOH (2 mL) was added P4O10 (0.5 g) at room temperature. The resulting suspension was stirred vigorously at 70° C. for 12 h. After completion, the mixture was diluted with water (20 mL), and extracted with EtOAc (3×20 mL). The combined organic layers were washed with water and brine, dried over Na2SO4 and evaporated to dryness. Flash chromatography (EtOAc-Hexane as eluent 1:1) afforded the title compound as viscous foam; Rf 0.28 (EtOAc-Hexane, 1:1, v/v); MS (ES+): 545 (M+H+).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07749992B2
Source datasetuspto-grants-2010_07
ORD IDord-d3c84ccb6b2a43359d290b26badacad7
Source noteuspto-grants-2010_07