반응 #486529

반응 방정식

ferrocene

N,N,N',N'-tetramethylethylenediamine

2,4,8,10-tetrakis(tert-butyl)-6-chloro-12H-dibenzo[d,g][1,3,2]dioxaphosphocin

n-butyl lithium

→

light brown solid

수율 58.5%

1,1'-Bis[2,4,8,10-tetrakis(tert-butyl)-12H-dibenzo[d,g][1,3,2]dioxaphosphocin-6-yl]ferrocene

수율 58.5%

용매

hexane

tetrahydrofuran

hexane

반응 조건

후처리

1. 1
   기타The residue is triturated with hexane
2. 2
   기타the resultant solid is recrystallized from an acetonitrile/tetrahydrofuran mixture

실험 절차

The general procedure of Example 1 is followed using 3.5 g (18.8 mmol) of ferrocene in 30 mL of hexane, 25 mL of a 1.6M hexane solution of n-butyl lithium, 4.5 g (38.7 mmol) of N,N,N',N'-tetramethylethylenediamine and 20 g (41 mmol) of 2,4,8,10-tetrakis(tert-butyl)-6-chloro-12H-dibenzo[d,g][1,3,2]dioxaphosphocin in 100 mL of tetrahydrofuran. The residue is triturated with hexane and the resultant solid is recrystallized from an acetonitrile/tetrahydrofuran mixture to give 12 g (58.5% yield) of a light brown solid.

출처