2-(2-氧代丙基)环己-1-one

反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of manganic acetate in acetic acid, prepared in situ by the addition of 16 g. of potassium permanganate (0.1 m.) to 88 g. of manganous acetate dihydrate (Mn(OAc)2. 2H2O) (0.42 m.) in 570 milliliters of glacial acetic acid followed by 124 ml. of acetic anhydride and 60 g. of potassium acetate, were added 100 g. (1.0 m.) of isopropenyl acetate and 98 g. (1.0 m.) of cyclohexanone. The reaction mixture was heated under nitrogen to 70° C. until the brown manganic color disappeared. The reaction mixture was cooled, diluted with water, and extracted with ether. The product, 2-acetonyl-cyclohexanone ##STR84## was isolated by distillation, b.p. 70° C. at 0.05 mm. mercury, yield about 8 g. (20% based on Mn). The reaction mixture was cooled extracted with ether

反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of manganic acetate in acetic acid, prepared in situ by the addition of 16 g. of potassium permanganate (0.1 m.) to 88 g. of manganous acetate dihydrate (Mn(OAc)2. 2H2O) (0.42 m.) in 570 milliliters of glacial acetic acid followed by 124 ml. of acetic anhydride and 60 g. of potassium acetate, were added 100 g. (1.0 m.) of isopropenyl acetate and 98 g. (1.0 m.) of cyclohexanone. The reaction mixture was heated under nitrogen to 70° C. until the brown manganic color disappeared. The reaction mixture was cooled, diluted with water, and extracted with ether. The product, 2-acetonyl-cyclohexanone ##STR84## was isolated by distillation, b.p. 70° C. at 0.05 mm. mercury, yield about 8 g. (20% based on Mn). The reaction mixture was cooled extracted with ether

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Following the general methods as outlined under Intermediate 13, starting from 2-(2-oxopropyl)cyclohexanone and 4-aminobenzoic acid, the title compound was isolated in 65% yield (98% purity by HPLC). MS(ESI+): 256.4; MS(ESI−): 254.4.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Following the general methods as outlined under Intermediate 7, starting from 2-(2-oxopropyl)cyclohexanone and 4-aminobenzoic acid, the title compound was isolated in 65% yield (98% purity by HPLC). MS(ESI+): 256.4; MS(ESI−): 254.4.

反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of manganic acetate in acetic acid, prepared in situ by the addition of 16 g. of potassium permanganate (0.1 m.) to 88 g. of manganous acetate dihydrate (Mn(OAc)2.2H2O) (0.42 m.) in 570 milliliters of glacial acetic acid followed by 124 ml. of acetic anhydride and 60 g. of potassium acetate, were added 100 g. (1.0 m.) of isopropenyl acetate and 98 g. (1.0 m.) of cyclohexanone. The reaction mixture was heated under nitrogen to 70° C. until the brown manganic color disappeared. The reaction mixture was cooled, diluted with water, and extracted with ether. The product, 2-acetonyl-cyclohexanone ##STR78## was isolated by distillation, b.p. 70° C. at .05 mm. mercury, yield about 8 g. (20% based on Mn). The reaction mixture was cooled extracted with ether

反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of manganic acetate in acetic acid, prepared in situ by the addition of 16 g. of potassium permanganate (0.1 m.) to 88 g. of manganous acetate dihydrate (Mn(OAc)2. 2H2O) (0.42 m.) in 570 milliliters of glacial acetic acid followed by 124 ml. of acetic anhydride and 60 g. of potassium acetate, were added 100 g. (1.0 m.) of isopropenyl acetate and 98 g. (1.0 m.) of cyclohexanone. The reaction mixture was heated under nitrogen to 70° C. until the brown manganic color disappeared. The reaction mixture was cooled, diluted with water, and extracted with ether. The product, 2-acetonyl-cyclohexanone ##STR84## was isolated by distillation, b.p. 70° C. at 0.05 mm. mercury, yield about 8 g. (20% based on Mn). The reaction mixture was cooled extracted with ether