Abstract: 4α,6α-bihydroxy-8α,9α-epoxy-1β-methylsulfony-2β,12-ether was obtained by methyl-sulfonylation from 1β,2β,4α,6α,8β,9α,12-hepthydroxy-β-dihydroagarofuran,a hydrolysis product of crude extract from Celastrus angulatus Max. and eight new β-dihydroagarofuran ether analogues were synthesized using 4α,6α-bihydroxy-8,9-epoxy-1β-methyl-sulfony-2β,12-ether-β-dihydroagarofuran as starting material.The structures of these compounds were comfirmed by NMR and MS spectral data.The preliminary bioassay results showed that compound 2.1~2.8 exhibited stomach toxicity against the third instar larvae of Mythimna separata and the mortality from derivative of allyl and n-butyl ether reached 66.7% and 50.0%,respectively at theconcentration of 20 mg/mL.