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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1184108Generated: November 2, 2026

Ethanol → tert-Butyl (3R,5S)-3-(hydroxymethyl)-5-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl)(2-methylpropyl)amino]piperidine-1-carboxylate

https://huagongshe.com/reaction/1184108

Reaction equation

Participants

RoleNameHCIDCharge
ReactantEthanolHCID 702—
ReactantSodium borohydrideHCID 4311764—
ReactantCalcium ChlorideHCID 5284359—
Reactant1-tert-Butyl 3-methyl(3R,5S)-5-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl}(2-methylpropyl)amino]piperidine-1,3-dicarboxylateHCID 58355550—
SolventWaterHCID 962—
SolventTetrahydrofuranHCID 8028—
SolventEthyl AcetateHCID 8857—
Producttert-Butyl (3R,5S)-3-(hydroxymethyl)-5-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl)(2-methylpropyl)amino]piperidine-1-carboxylateHCID 5835567247.4%

Reaction Conditions

Temperature0 °C

Reaction Steps

Sodium borohydride (4.45 g) was suspended in THF (25 ml)-ethanol (75 ml), and calcium chloride (6.5 g) was added. After stirring at 0° C. for 1 hr, a solution of 1-tert-butyl 3-methyl (3R,5S)-5-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl}(2-methylpropyl)amino]piperidine-1,3-dicarboxylate (4.0 g) in THF (50 ml) was added. After stirring at room temperature for 12 hr, ethyl acetate (150 ml) and water (50 ml) were slowly added in this order, and the mixture was filtered. The organic layer of the filtrate was partitioned, washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was dried under reduced pressure to give the object product (1.8 g).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08664380B2
Source datasetuspto-grants-2014_03
ORD IDord-c0634a9778b14e1cb22b7c671185e234
Source noteuspto-grants-2014_03