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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 450816Generated: October 31, 2026

Sodium sulfate decahydrate → HCID 72303498, compound

https://huagongshe.com/reaction/450816

Reaction equation

Participants

RoleNameHCIDCharge
ReactantSodium sulfate decahydrateHCID 62649—
ReactantAluminium lithium hydrideHCID 21226445—
ReactantHCID 72303307HCID 72303307—
SolventTetrahydrofuranHCID 8028—
ProductHCID 72303498HCID 7230349828.2%

Reaction Conditions

Temperature0 °C

Reaction Steps

To a solution of 600 mg of methyl 5-{[({[(3RS,4RS)-3-(2,4-dichlorophenyl)-2-{(1SR,2SR)-2-[(methylsulfonyl)amino]cyclohexyl}-1-oxo-1,2,3,4-tetrahydroisoquinolin-4-yl]carbonyl}amino)oxy]methyl}thiophene-3-carboxylate in 40 mL of THF was added 45 mg of lithium aluminum hydride at −78° C. The solution was warmed to 0° C., followed by stirring for 3 hours. Sodium sulfate decahydrate was added thereto, followed by stirring for 1 hour. After removing sodium sulfate by filtration, the organic layer was dried by adding anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform-methanol) to obtain 162 mg of (3RS,4RS)-3-(2,4-dichlorophenyl)-N-{[4-(hydroxymethyl)-2-thienyl]methoxy}-2-{(1SR,2SR)-2-[(methylsulfonyl)amino]cyclohexyl}-1-oxo-1,2,3,4-tetrahydroisoquinoline-4-carboxamide as a white solid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08486970B2
Source datasetuspto-grants-2013_07
ORD IDord-4430ddfffdef4da88dac75e30f997d37
Source noteuspto-grants-2013_07