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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 228491Generated: October 30, 2026

1,2-Dichloroethane → HCID 59730339, compound

https://huagongshe.com/reaction/228491

Reaction equation

Participants

RoleNameHCIDCharge
Reactant1,2-DichloroethaneHCID 11—
ReactantCitric AcidHCID 311—
Reactant1-HydroxybenzotriazoleHCID 75771—
ReactantDiisopropylethylamineHCID 81531—
ReactantSodium BicarbonateHCID 516892—
ReactantMethylamine hydrochlorideHCID 6364545—
ReactantHCID 59730271HCID 59730271—
SolventDichloromethaneHCID 6344—
ProductHCID 59730339HCID 5973033963%

Reaction Steps

Combine 6-(4-{[tert-Butoxycarbonyl-(3-methyl-butyl)-amino]-methyl}-phenoxy)-nicotinic acid (0.090 g, 0.21 mmol), CH2Cl2 (5 mL), EDC (0.048 g, 0.25 mmol), HOBt (0.034 g, 0.25 mmol), Hunig's Base (92 uL, 0.53 mmol), and Methylamine Hydrochloride (0.014 g, 0.21 mmol) in a 7 mL reaction vial. After reactions shake for 72 hours, add 10% Citric acid, followed by 10% NaHCO3, and then add the organic mixture to a Celite column. Elute with CH2Cl2, concentrate, and flash chromatograph using 2:1 Ethyl acetate:Hexanes eluent to afford 56.2 mg (63% yield) of the title compound: 1H NMR (500 MHz, CDCl3); 0.9 (6H, d), 1.3-1.6 (12H, m), 3.0 (3H, s), 3.1-3.3 (2H, m), 4.3-4.5 (2H, m), 6.3 (1H, br s), 6.9 (1H, d), 7.1 (2H, d), 7.2-7.4 (2H, m), 8.1 (1H, d), 8.5 (1H, s); MS m/z 328 (M−100, Boc).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07560463B2
Source datasetuspto-grants-2009_07
ORD IDord-a9df2c513c2745a9871849e5df75eeee
Source noteuspto-grants-2009_07