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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1045585Generated: October 31, 2026

Potassium Phosphate, Tribasic → HCID 59368144, compound

https://huagongshe.com/reaction/1045585

Reaction equation

Participants

RoleNameHCIDCharge
ReactantPotassium Phosphate, TribasicHCID 62657—
ReactantMorpholine, 4-(chloroacetyl)-HCID 74040—
ReactantL-ProlineHCID 145742—
Reactant1,2,3,4,5,6-Hexahydro-3,9-dimethylazepino[4,5-b]indoleHCID 68560092—
CatalystCopper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)HCID 24350—
SolventDimethylformamideHCID 6228—
ProductHCID 59368144HCID 593681442.5%

Reaction Steps

The title compound was prepared by following general procedure 7. 3,9-Dimethyl-1,2,3,4,5,6-hexahydroazepino[4,5-b]indole (100 mg, 0.46 mmol), was taken into DMF. To the above solution CuI (9 mg, 0.046 mmol), L-proline (11 mg, 0.093 mmol), K3PO4 (198 mg, 0.93 mmol) were added and stirred for 10 min. at RT. 2-Chloro-1-morpholinoethanone (91 mg, 0.56 mmol) was added dropwise. The reaction mixture was heated at 90° C. for 12 h. After completion of reaction, the reaction mixture was filtered through Celite. DMF was evaporated under reduced pressure and then extracted with ethyl acetate. The organic layer was dried over Na2SO4, and concentrated under reduced pressure. To obtain 4 mg of 2-(3,9-dimethyl-2,3,4,5-tetrahydroazepino[4,5-b]indol-6(1H)-yl)-1-morpholinoethanone as the TFA salt after purification by reverse-phase chromatography (C-18, 500 mm×50 mm, Mobile Phase A=0.05% TFA in water, B=0.05% TFA in acetonitrile, Gradient: 10% B to 80% B in 30 min., injection vol. 5 mL).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08569287B2
Source datasetuspto-grants-2013_10
ORD IDord-ff54f2701d0c437dbff6a7618c4ea0e9
Source noteuspto-grants-2013_10