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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1915989Generated: November 1, 2026

Diethylamine → HCID 45111295, compound

https://huagongshe.com/reaction/1915989

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDiethylamineHCID 8021—
ReactantOxalyl chlorideHCID 65578—
ReactantDiisopropylethylamineHCID 81531—
Reactant4-Methyl-1,2-dithiolane-4-carboxylic acidHCID 20069311—
SolventDimethylformamideHCID 6228—
SolventDichloromethaneHCID 6344—
SolventEthylacetate heptaneHCID 21899848—
ProductHCID 45111295HCID 45111295—

Reaction Conditions

Temperature0 °C

Reaction Steps

5 ml of anhydrous dichloromethane and 0.1 ml of anhydrous DMF are added to 2.26 mmol of Compound 1. The mixture is cooled to 0° C. and 2.7 mmol of oxalyl chloride are added. The mixture is stirred at 20° C. and then added at 0° C. to a mixture of 2.26 mmol of diethylamine, 5 ml of anhydrous dichloromethane and 6.8 mmol of diisopropylethylamine. The reaction medium is stirred for 3 hours at 20° C. When the reaction is complete, the medium is diluted in 50 ml of dichloromethane and then washed with 2×30 ml of water and 1×50 ml of saturated NH4Cl solution, dried over Na2SO4 and evaporated to dryness on a rotavapor. After flash chromatography (eluent: heptane/EtOAc), Compound 18 is isolated in the form of a yellow oil (48% yield).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08617524B2
Source datasetuspto-grants-2013_12
ORD IDord-91ea94b8d4124a3dbed2cbc620bf0ce1
Source noteuspto-grants-2013_12