Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2356144Generated: November 2, 2026

Sodium hydride → HCID 22730180, compound

https://huagongshe.com/reaction/2356144

Reaction equation

Participants

RoleNameHCIDCharge
ReactantSodium hydrideHCID 24758—
Reactant15-Crown-5HCID 36336—
ReactantTert-butyl 3-oxopiperazine-1-carboxylateHCID 3157178—
ReactantHCID 22730382HCID 22730382—
SolventWaterHCID 962—
SolventDimethylformamideHCID 6228—
ProductHCID 22730180HCID 22730180—

Reaction Conditions

Temperature60 °C

Reaction Steps

A solution of Example 500B (328 mg, 1.64 mmol) in DMF (4 mL) at room temperature was treated with 15-crown-5 (361 mg, 1.64 mmol) and 60% sodium hydride in mineral oil (66 mg, 1.64 mmol). The mixture was treated with a solution of Example 500C (500 mg, 1.49 mmol) in DMF (2 mL), heated to 60° C. for 16 hours, cooled to room temperature, treated with water (20 mL), and extracted three times with ethyl acetate (50 mL). The combined extracts were washed with brine (10 mL), dried (Na2SO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 1:1 ethyl acetate/hexanes to provide the desired product.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07754886B2
Source datasetuspto-grants-2010_07
ORD IDord-be3747ac5ddf47fca90a7da868fbb5c0
Source noteuspto-grants-2010_07