تفاعل #450241

معادلة التفاعل

diisopropylazodicarboxylate

4-(3,3-dichloro-2-propenyloxy)-2,6-dichlorophenol

m-phenoxybenzyl alcohol

triphenylphosphine

→

3,5-dichloro-4-(3-phenoxybenzyl)-1-(3,3-dichloro-2-propenyloxy)-benzene

المردود 59.6%

المذيبات

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGAfter stirring at room temperature for 12 hours
2. 2
   تركيزthe reaction mixture was concentrated
3. 3
   workup.ADDITIONmixed with 20 ml of diethyl ether
4. 4
   ترشيحThe precipitate was filtered
5. 5
   تركيزthe filtrate was concentrated

الإجراء التجريبي

To a solution of 0.33 g of 4-(3,3-dichloro-2-propenyloxy)-2,6-dichlorophenol, 0.23 g of m-phenoxybenzyl alcohol and 0.34 g of triphenylphosphine dissolved in 10 ml of tetrahydrofuran was added dropwise a solution of 0.26 g of diisopropylazodicarboxylate dissolved in 5 ml of tetrahydrofuran, while stirring at room temperature. After stirring at room temperature for 12 hours, the reaction mixture was concentrated, and then mixed with 20 ml of diethyl ether. The precipitate was filtered, and the filtrate was concentrated. The residue was subjected to silica gel chromatography, which afforded 0.31 g of 3,5-dichloro-4-(3-phenoxybenzyl)-1-(3,3-dichloro-2-propenyloxy)-benzene (57% yield), nD25.5 1.6066.

المصدر