HCID 21850811, compound → HCID 178454802, compound

Participants

Reaction Conditions

Reaction Steps

The methyl (1-hydroxy-1-methylethyl)phosphinate prepared as described immediately above is heated with water (11) on a steam bath for 8 hours until conversion to 1-hydroxy-1-methylethylphosphonous acid is complete (monitored by 31P nmr). The water is removed on a rotary evaporator and the residue is completely dried by co-evaporation with toluene. A sample of this phosphonous acid (4.6 g, 0.037M), isobutyl alcohol (3.02 g, 0.041M) and dimethylaminopyridine (0.5 g, 0.0041M) is stirred at 5° C. in tetrahydrofuran. Dicyclohexylcarbodiimide (8.4 g, 0.041M) is added portionwise over 30 minutes. On completion of the reaction (31P nmr), ether (50 ml) is added and the precipitated dicyclohexyl urea is filtered off.

Provenance & Evidence