反应详情

6-amino-5-oxohexanoic acid hydrochloride (S1) 22.44 g (0.12 mol) (Lartillot, Serge. et al, Bulletin de la Societe Chimique de France, 1964, 4:783) was solved in about 6.1 L sodium dihydrogen phosphate buffer (300 g sodium dihydrogen phosphate was solved in 6 L water, then Saturated sodium hydroxide aqueous solution was added until a pH of about 6.5 was reached), and ethyl acetoacetate 16.12 g (0.12 mol) was added to the above-mentioned solution. The reaction solution was refluxed for half an hour, cooled to room temperature and Na2CO3 was added until a pH of about 8 was reached. The mixture was extracted with 100 ml CHCl3 and Aqueous phase was acidified with 6 mol/L HCl to pH 1. The brown solid was collected by filtration, washed with water and dried in vacuum condition to give 20.29 g (71%) 4-(4-(ethoxycarbonyl)-5-methyl-1H-pyrrol-3-yl)butanoic acid (S2).

1. additionwas added to the above-mentioned solution
2. temperatureThe reaction solution was refluxed for half an hour
3. extractionThe mixture was extracted with 100 ml CHCl3 and Aqueous phase
4. filtrationThe brown solid was collected by filtration
5. washwashed with water
6. customdried in vacuum condition