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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 645382Generated: October 30, 2026

Water → HCID 86613106, compound

https://huagongshe.com/reaction/645382

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantTrifluoromethanesulfonic acidHCID 62406—
ReactantSelectfluorHCID 2724933—
ReactantN-trifluoroacetyl-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepineHCID 22292806—
Solvent1,2-DichloroethaneHCID 11—
ProductHCID 86613106HCID 8661310622.8%

Reaction Conditions

Temperature75 °C

Reaction Steps

A solution of N-trifluoroacetyl-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (2.5 g, 8.5 mmol) in 1,2-dichloroethane (15 mL) was treated with Selectfluor (3.9 g, 11 mmol), trifluoromethanesulfonic acid (8 mL, 90 mmol) and stirred 60 hours at 75° C. The product mixture was poured into water (200 mL), extracted with EtOAc (200 mL), the organic phase washed with saturated aqueous NaHCO3 (2×100 mL), brine (100 mL), dried with Na2SO4 and concentrated. The crude product was purified by flash chromatography (6% EtOAc in hexane, silica) resulting in 0.6 g of a white solid. MS calculated for C13H12ClF4NO+H: 310, observed: 310.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07704993B2
Source datasetuspto-grants-2010_04
ORD IDord-ea74f8ce43b14449871b13c0777475fa
Source noteuspto-grants-2010_04