s 1h 7 95 d j 14 7 hz 1h 7 24 t j 8 9 hz 1h 5 19 5 11 m 1h 4 82 4 72 m 2h 4 39 4 27 m 2h 4 35 q j 7 5 hz 2h 3 19 s 3h 2 57 sept j 7 1 hz 1h 1 36 t j 7 4 hz 3h 1 17 d j 7 1 hz 6h 1 18 s 9h a suspension of example 8c 110 kg and n chlorosuccinimide 31 kg in ethyl acetate 785 kg at 0 5 u00b0 c was treated with phosphoric acid 2 5 kg and water 1 kg while the temperature was kept at less than 5 u00b0 c warmed to 22 u00b0 c stirred for 3 hours washed with sodium bicarbonate solution and 10 sodium sulfite solution and concentrated the concentrate was treated with methyl tert butyl ether 403 kg and the slurry was stirred at 35 u00b0 c for 30 minutes cooled to 5 u00b0 c and filtered a suspension of example 8c 4 91 g and n chlorosuccinimide 1 36 g in ethyl acetate 500 ml was treated with trifluoroacetic acid 0 15 ml over 3 hours then with 5 aqueous sodium bicarbonate 25 ml separated from the water layer washed with 10 aqueous sodium hydrogen sulfate 10 ml and concentrated to 50 ml with a methyl tert butyl ether 250 ml azeotrope the concentrate was dissolved in methyl tert butyl.