Dabco → HCID 86760543, compound

Participants

Reaction Conditions

Reaction Steps

2.5 g (7.9 mmol) of the thus obtained 2-bromobenzyl(di-tert-butyl)phosphine, 2.24 g DABCO (20 mmol), 1.94 g 1,3,5-trimethyl-4,6,9-trioxa-2-phosphatricyclo[3.3.1.1{3,7}]decane (9 mmol) and 0.23 g Pd(PPh3)4 (0.2 mmol) in 10 ml toluene were added into a 250 ml glass vessel under inert atmosphere, and the content of the vessel was heated to 140° C. under stirring for 12 hours. The mixture was than allowed to cool to 100° C., and was then filtered. The filtrate was cooled to room temperature, then 30 ml of methanol added were added and the mixture cooled for a period for 12 hours to −35+ C., 8-(2-{[di(tert-butyl)-phosphino]-methyl}phenyl)-1,3,5,7-tetramethyl-2,4,6-trioxa-8-phosphatricyclo[3.3.1.1{3,7}]decane was isolated as yellow crystals (2.2 g, 4.9 mmol, 62%), and could be characterized by showing two distinct resonance signals in 31P NMR at +38.08 and −38.96 ppm.

Provenance & Evidence