87 1 92 m 1h 1 32 1 42 m 1h 1 30 d j 5 92 hz 3h 1 30 1 25 m 6h 0 98 qt j 15 7 3 18 hz 2h ms esi m 1 m z calculated 340 found 340 to a 10 l three necked round bottomed flask equipped with an agitator thermometer and a nitrogen inlet tube was added 200 g of compound 8 1 07 mol from synergetica philadelphia pa thf 1000 ml was added to dissolve compound 8 after the solution was cooled to u2212 80 u00b0 c to u2212 50 u00b0 c 2 0 m lda in hexane thf 1175 ml 2 2 eq was added while maintaining the batch temperature below u2212 50 u00b0 c after about 15 minutes of agitation at u2212 80 u00b0 c to u2212 50 u00b0 c diethyl chlorophosphate 185 ml 1 2 eq was added while maintaining the batch temperature below u2212 50 u00b0 c the mixture was agitated at a temperature from u2212 80 u00b0 c to u2212 50 u00b0 c for about 15 minutes and diluted with n heptane 1000 ml this mixture was warmed up to about u2212 35 u00b0 c and quenched with aqueous ammonium chloride 400 g in 1400 ml water at a temperature below u2212 10 u00b0 c this mixture was.