반응 #471643

반응 방정식

1,4-dioxaspiro[4.5]dec-8-ylmethanol

3-(benzyloxy)phenol

triphenylphosphine

→

8-{[3-(benzyloxy)phenoxy]methyl}-1,4-dioxaspiro[4.5]decane

수율 47.8%

용매

THF

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타The reaction liquid
3. 3
   농축was concentrated under reduced pressure, benzene
4. 4
   workup.ADDITIONwas added to the residue, and insolubles
5. 5
   기타were removed by filtration
6. 6
   농축The filtrate was concentrated under reduced pressure
7. 7
   기타the residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=92/8-85/15)

실험 절차

To a solution of 1,4-dioxaspiro[4.5]dec-8-ylmethanol (946 mg), 3-(benzyloxy)phenol (1 g), and triphenylphosphine (1.57 g) in THF (15 mL) was added azodicarboxylate diethyl (944 μL) under ice-cooling, and the mixture was stirred at room temperature overnight. The reaction liquid was concentrated under reduced pressure, benzene was added to the residue, and insolubles were removed by filtration. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=92/8-85/15) to obtain 8-{[3-(benzyloxy)phenoxy]methyl}-1,4-dioxaspiro[4.5]decane (846 mg).

출처