Sodium hydride → 6-{[2,4,8,10-Tetra-tert-butyl-12-methyl-dibenzo[d,g][1,3,2]dioxaphosphocin-6-yl]oxy}-2,4,8,10-tetra-tert-butyl-12-methyl-dibenzo[d,g][1,3,2]dioxaphosphocin

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Reaction Steps

To a solution of 17.3 g (36 mmol) of the compound of Example 8 in 250 mL of dry tetrahydrofuran (THF) is added 1.0 g (41 mmol) of sodium hydride at 3° C. After the addition is complete, the reaction mixture is allowed to warm to room temperature. The reaction mixture is stirred for 14 hours at ambient temperature. To the reaction mixture is then added 14.8 g(29 mmol) of the compound of Example 7 at ambient temperature. After 48 hours, the reaction mixture is filtered and the filtrate is concentrated under vacuum. The residue is purified by flash chromatography with 1% ethyl acetate/99% hexane to give the tide compound as a white solid melting at 281°-285° C.

Provenance & Evidence