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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1041224Generated: November 2, 2026

Isopropanol → HCID 178425838, compound

https://huagongshe.com/reaction/1041224

Reaction equation

Participants

RoleNameHCIDCharge
ReactantIsopropanolHCID 3776—
ReactantBicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-HCID 18462—
Reactant7-Amino-5,5-dimethyl-1,3,4,5-tetrahydro-benzo[b]azepin-2-oneHCID 57853830—
ReactantHCID 178506249HCID 178506249—
ProductHCID 178425838HCID 17842583826.5%

Reaction Steps

(2,5-Dichloro-pyrimidin-4-yl)-[2-(4-trifluoromethyl-1H-imidazol-2-yl)-phenyl]-amine (50.0 mg, 0.134 mmol), 7-Amino-5,5-dimethyl-1,3,4,5-tetrahydro-benzo[b]azepin-2-one (27.0 mg, 0.132 mmol) and 10-Camphorsulfonic acid (31.0 mg, 0.133 mmol) were suspended in Isopropyl alcohol (3.0 mL, 0.039 mol) and the reaction was microwaved on 300 watts, 140° C. for 20 minutes. The reaction mixture was then reduced under nitrogen and the crude residue was isolated and purified by prep HPLC to afford 18.95 mg (26%) of the desired product as a TFA salt. LC/MS (ESI): 558.26. 1H NMR (400 MHz, DMSO, d6) δ 9.46 (s, 1H), 9.39 (s, 1H), 8.96 (m, 1H), 8.23 (s, 1H), 8.08 (s, 1H), 7.97 (m, 1H), 7.66 (m, 1H), 7.54 (m, 1H), 7.39 (m, 1H), 7.21 (m, 1H), 6.91 (d, 1H, J=8.59 Hz), 2.16 (m, 2H), 1.98 (m, 2H), 1.29 (s, 6H).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08552186B2
Source datasetuspto-grants-2013_10
ORD IDord-886efe8832fb49f09264ef87369f5836
Source noteuspto-grants-2013_10