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With sodium hydroxide In methanol; water for 0.5 h; Reflux
265·6g intermediate III and 60. 8g of sodium hydroxide in 200ml of methanol and 1328ml of water was heated at reflux for about 30min, and then concentrated under reduced pressure, the concentrate was added 450ml of water, 500ml of methylene chloride was stirred stationary layers were separated aqueous layer was added diethyl chloride 1300ml, then a solution of concentrated hydrochloric acid ΡΗ = 1~2, the organic phase was washed with water until neutral, concentrated under reduced pressure, the residue was added ethyl acetate 2L crystallization, filtration after 2h Yang Jing, receipts 203g. Take 200g resulting solid was added to 330ml of ethyl acetate, heated clear solution was added active carbon reflux, filtration, the filtrate was added ethyl acetate at room temperature crystallization, filtration as white crystals 181g, purity of 99.81percent.
With dicyclohexyl-carbodiimide; In dichloromethane; at 20.0℃; for 4.0h;
2 g of <strong>[30299-08-2]2,2'-(cyclohexylidene-bis(p-phenyleneoxy))bis(2-methylbutyric acid)</strong>, 1.2 g of dicyclohexylcarbodiimide, 0.6 g of 2-amino-1-(4-hydroxyphenyl)ethyl ketone and 60 ml of dichloromethane were placed into the 100 ml single-neck flask, reacted for 4 hours at room temperature, evaporated to dryness, then purified through chromatography on silica gel column, to give the target compound (2.16 g). MS (ESI): 588 (M+H+).
With dicyclohexyl-carbodiimide; In dichloromethane; at 20.0℃; for 4.0h;
4 g of <strong>[30299-08-2]2,2'-(cyclohexylidene-bis(p-phenyleneoxy))bis(2-methylbutyric acid)</strong>, 2.48 g of dicyclohexylcarbodiimide, 0.6 g of 2-amino-1-(4-hydroxyphenyl)ethyl ketone and 60 ml of dichloromethane were placed into the 100 ml single-neck flask, reacted for 4 hours at room temperature, evaporated to dryness, then purified through chromatography on silica gel column, to give the target compound (3.56 g). MS (ESI): 707 (M+H+).
With dicyclohexyl-carbodiimide; In dichloromethane; at 20.0℃; for 4.0h;
Experiment 11 Preparation of Compound 11 [0088] 2 g of 2,2?-(cyclohexylidene-bis(p-phenyleneoxy))bis(2-methylbutyric acid), 1.2 g of dicyclohexylcarbodiimide, 0.6 g of 2-amino-1-(4-hydroxyphenyl)ethyl ketone and 60 ml of dichloromethane were placed into the 100 ml single-neck flask, reacted for 4 hours at room temperature, evaporated to dryness, then purified through chromatography on silica gel column, to give the target compound (2.16 g). MS (ESI): 588 (M+H+).
With dicyclohexyl-carbodiimide; In dichloromethane; at 20.0℃; for 4.0h;
Experiment 12 Preparation of Compound 12 [0089] 4 g of 2,2?-(cyclohexylidene-bis(p-phenyleneoxy))bis(2-methylbutyric acid), 2.48 g of dicyclohexylcarbodiimide, 0.6 g of 2-amino-1-(4-hydroxyphenyl)ethyl ketone and 60 ml of dichloromethane were placed into the 100 ml single-neck flask, reacted for 4 hours at room temperature, evaporated to dryness, then purified through chromatography on silica gel column, to give the target compound (3.56 g). MS (ESI): 707 (M+H+).
With sodium hydroxide; In methanol; water; for 0.5h;Reflux;
265·6g intermediate III and 60. 8g of sodium hydroxide in 200ml of methanol and 1328ml of water was heated at reflux for about 30min, and then concentrated under reduced pressure, the concentrate was added 450ml of water, 500ml of methylene chloride was stirred stationary layers were separated aqueous layer was added diethyl chloride 1300ml, then a solution of concentrated hydrochloric acid RhoEta = 1~2, the organic phase was washed with water until neutral, concentrated under reduced pressure, the residue was added ethyl acetate 2L crystallization, filtration after 2h Yang Jing, receipts 203g. Take 200g resulting solid was added to 330ml of ethyl acetate, heated clear solution was added active carbon reflux, filtration, the filtrate was added ethyl acetate at room temperature crystallization, filtration as white crystals 181g, purity of 99.81%.