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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1585332Generated: November 3, 2026

Lithium Hexamethyldisilazide → 5(S)-[1(S)-(Boc-amino)-2-phenylethyl]-3(R)-[(p-benzyloxyphenyl)methyl]dihydrofuran-2-(3H)-one

https://huagongshe.com/reaction/1585332

Reaction equation

Participants

RoleNameHCIDCharge
ReactantLithium HexamethyldisilazideHCID 2733832—
Reactanttert-butyl(1S)-1-[(2S)-5-oxotetrahydrofuran-2-yl]-2-phenylethylcarbamateHCID 10870461—
Reactantp-Benzyloxybenzyl iodideHCID 11723738—
ReactantEthyl acetate hexaneHCID 21226206—
SolventTetrahydrofuranHCID 8028—
Solvent2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-HCID 81646—
Product5(S)-[1(S)-(Boc-amino)-2-phenylethyl]-3(R)-[(p-benzyloxyphenyl)methyl]dihydrofuran-2-(3H)-oneHCID 15659556—

Reaction Steps

In analogy with Example 1h), 1.13 g (3.70 mmol) of 5(S)-[1(S)-(Boc-amino)-2-phenylethyl]dihydrofuran-2-(3H)-one [Example 2b)], dissolved in 4.8 ml of THF and 0.75 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone, are deprotonated, at -75° C., with 7.25 ml of a 1M solution of lithium bis(trimethylsilyl)amide in THF, and alkylated (15 min) with 1.2 g (3.7 mmol) of p-benzyloxybenzyl iodide (Example 1d)) in 2 ml of THF. Column chromatography (SiO2, hexane/ethyl acetate, 2:1) affords the pure title compound: TLC Rf (D)=0.30; tRet (I)=28.2 min; FAB-MS (M+H)+ =502.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05935976
Source datasetuspto-grants-1999_08
ORD IDord-7a3fc637d0754d43b5cbeaa68b2d7a6f
Source noteuspto-grants-1999_08