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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1754489Generated: October 28, 2026

Sodium Iodide → HCID 67219209, compound

https://huagongshe.com/reaction/1754489

Reaction equation

Participants

RoleNameHCIDCharge
ReactantSodium IodideHCID 5238—
Reactant2-((1,1-Dimethylethyl)imino)-N,N-diethylhexahydro-1,3-dimethyl-2lambda5-1,3,2-diazaphosphorin-2-amineHCID 3513851—
Reactant774239-48-4HCID 43141455—
Reactantmethyl 2-(2-methyl-1H-pyrrolo[2,3-b]pyridin-3-yl)acetateHCID 67218699—
SolventWaterHCID 962—
SolventDimethylformamideHCID 6228—
SolventDiethylether ethylacetateHCID 21584169—
ProductHCID 67219209HCID 67219209—

Reaction Steps

A solution of (2-methyl-1H-pyrrolo[2,3-b]pyridin-3-yl)-acetic acid methyl ester ((2.37 g, 11.12 mmol) in dry DMF (38 ml) at room temperature is treated with BEMP (4.39 ml, 15.19 mmol) dropwise. The reaction mixture is stirred at room temperature for 35 minutes and then 1-(1-bromo-ethyl)-4-methanesulfonyl-benzene (4.00 g, 15.18 mmol) and sodium iodide (12.29 g, 15.28 mmol) is added. After stirring at 60° C. for 1 hour, the reaction mixture is allowed to cool to room temperature and then diluted with ethyl acetate/ether (200 ml of a 1:1 mixture) and water (150 ml). The organic portion is washed with brine, dried (Na2SO4) and concentrated in vacuo and the resulting crude is purified by chromatography on silica eluting with ethyl acetate/iso-hexane (2:3 increasing to 1:1 ethyl acetate) to yield the titled product as a racemic mixture. The enantiomers are resolved using a chiralcel OD column eluting with 30% IPA in hexanes to afford enantiomer A (retention time=14.33 minutes) and enantiomer B (retention time=17.68 minutes)

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09169251B2
Source datasetuspto-grants-2015_10
ORD IDord-970ffafa17484e02b1d6eb8323f9de20
Source noteuspto-grants-2015_10