Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1630508Generated: October 30, 2026

Triethylamine → HCID 68283735, compound

https://huagongshe.com/reaction/1630508

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTriethylamineHCID 8471—
ReactantEthyl chloroformateHCID 10928—
ReactantHCID 68284096HCID 68284096—
SolventDichloromethaneHCID 6344—
ProductHCID 68283735HCID 6828373545.9%

Reaction Steps

To a stirred solution of 2-(1,2,3,4-tetrahydro-8-methylpyrido[4,3-b]indol-5-yl)-1-(pyridin-4-yl)ethanol (300 mg, 0.977 mmol) and triethyl amine (0.18 mL, 1.27 mmol) in DCM (6 mL) was added ethyl chloroformate (138 mg, 1.27 mmol), and the reaction mixture stirred at RT for 2 h. The progress of reaction was monitored by TLC and LCMS. The reaction mixture was diluted with DCM and washed with water. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH-DCM) to yield ethyl 3,4-dihydro-5-(2-hydroxy-2-(pyridin-4-yl)ethyl)-8-methyl-1H-pyrido[4,3-b]indole-2(5H)-carboxylate (170 mg). 1H NMR (CDCl3, freebase) δ (ppm): 8.4 (d, 2H), 7.21 (m, 4H), 7.0 (d, 1H), 5.03 (t, 1H), 4.6 (m, 2H), 4.21 (m, 4H), 3.78 (m, 2H), 3.6 (m, 1H), 2.75 (m, 1H), 2.4 (s, 3H), 1.28 (t, 3H). Separation by chiral HPLC provides enantiomers 72a and 72b.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08791132B2
Source datasetuspto-grants-2014_07
ORD IDord-906120cf46f14abab06506f55578842f
Source noteuspto-grants-2014_07