Triethylamine → HCID 18459669, compound

HRID 2302143Notes

Reaction equation

C(N(CC)CC)C.[CH3:8][S:9](Cl)(=[O:11])=[O:10].[Cl:13][C:14]1[C:19]([Cl:20])=[CH:18][C:17]([OH:21])=[CH:16][N:15]=1>C(Cl)Cl>[Cl:13][C:14]1[C:19]([Cl:20])=[CH:18][C:17]([O:21][S:9]([CH3:8])(=[O:11])=[O:10])=[CH:16][N:15]=1

Participants

Conditions

Temperature: 20 °C

Procedure

At 0° C., initially 7.9 g of triethylamine and then 8.5 g of methanesulfonyl chloride were added to 11.6 g of 2,3-dichloro-5-hydroxypyridine in 150 ml of methylene chloride. The mixture was subsequently stirred at approximately 20° C. for 17 hours and then washed with 100 ml of water. The organic phase was dried over magnesium sulfate and then concentrated. The resulting crude product was purified by silica gel chromatography (mobile phase: ethyl acetate/cyclohexane (1:1)). Yield: 9.1 g.

Workup

washwashed with 100 ml of water
dry with materialThe organic phase was dried over magnesium sulfate
concentrationconcentrated
customThe resulting crude product was purified by silica gel chromatography (mobile phase: ethyl acetate/cyclohexane (1:1))

Sources & evidence

ORD record: ord-d2f64d340e824bbeacca7ccb4f0c1dde
Source dataset: uspto-grants-2002_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06432880B1

Reaction notes

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