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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 351578Generated: October 30, 2026

Acetic Acid → HCID 22556753, compound

https://huagongshe.com/reaction/351578

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAcetic AcidHCID 176—
ReactantAllylamineHCID 7853—
Reactant1,3,4,5-Tetrahydro-2H-1-benzazepin-2-oneHCID 248580—
ReactantSodium triacetoxyborohydrideHCID 5049666—
Solvent1,2-DichloroethaneHCID 11—
SolventDichloromethaneHCID 6344—
ProductHCID 22556753HCID 2255675382%

Reaction Conditions

Temperature22 °C

Reaction Steps

To a solution of indole-7-carboxaldehyde 1 (4.00 g, 27.6 mmol) in 1,2-dichloroethane (120 mL) at 20-24° C. was added allylamine (2.50 mL, 33.1 mmol), acetic acid (3.4 mL), and sodium triacetoxyborohydride (5.85 g, 27.6 mmol). The resulting mixture was stirred at 20-24° C. for 5 hours. An additional 1.5 g (7.1 mmol) of sodium triacetoxyborohydride was added and the resulting mixture was stirred overnight. The mixture was diluted with dichloromethane (300 mL), washed carefully with aqueous sodium bicarbonate (100 mL), and the layers were separated. The organic layer was washed with water (100 mL), saturated aqueous sodium chloride (100 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, eluting with 10-30% ethyl acetate in hexanes. Fractions containing product were combined and concentrated under reduced pressure to provide 4.21 g (82%) of the desired compound as a light yellow oil.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06743785B2
Source datasetuspto-grants-2004_06
ORD IDord-88c6d581ec40428ea215c7cac3270052
Source noteuspto-grants-2004_06