the reaction mixture in comparison with the standard initially sampled the reaction was continued and sampling repeated until the amount of bp relative to standard was u2266 0 5 area the reaction mixture was concentrated under vacuum by distillation with the reaction mixture maintained at a temperature of from 35 u00b0 c to 45 u00b0 c to a volume of 600 ml forming a thick slurry nmp 280 ml was then added to the reaction mixture and it was further concentrated under the batch under vacuum by distillation with the reaction mixture maintained at a temperature of from 35 u00b0 c to 45 u00b0 c to a volume of about 560 ml forming a clear solution this solution was used directly in the part b coupling step into a 1 l 3 neck round bottom flask was placed 320 ml of etoac and dissolved therein 80 g of compound 9 166 mmol 1 eq 28 g hobt h 2 o 182 mmol 1 1 eq and 48 g edcl hcl 250 mmol 1 4 eq in nmp 320 ml the reaction mixture was stirred for 40 minutes while maintaining the reaction mixture at a temperature of 25 u00b0 c the entire amount of the solution of bp prepared in part a above was added to the reaction mixture with stirring the reaction mixture was stirred for 10 min and 80 ml of n methyl morpholine 724 mmol 4 4 eq was added to reaction at a rate which.