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cis-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol[ No CAS ]
trans-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
0.6 g; 1.2 g
With potassium carbonate; In N,N-dimethyl-formamide; at 20℃;
Step 5: synthesis of cis-4- [(4-chloro-2-nitrophenyl)amino] -1 -methylcyclohexanol A mixture of <strong>[233764-32-4]4-amino-1-methylcyclohexanol</strong> (2.9 g, 22.3 mmol), 4-chloro-1-fluoro-2-nitro- benzene (3.9 g, 22.3 mmol) and K2C03 (9.2 g, 66.9 mmol) in DMF (40 mL) was stined under argon at RT overnight. The resulting mixture was diluted with EA (200 mL) and then washed by saturated NH4C1 solution. The resulting organic layer was concentrated in vacuo. The residuewas purified by column chromatography on silica gel (EA: PE = 1:19 to 1:4) to afford 0.6 g of cis-4- [(4-chloro-2-nitrophenyl)amino] -1 -methylcyclohexanol, 1.2 g of trans-4- [(4-chloro-2- nitrophenyl)amino]-1-methylcyclohexanol, and 3.2 g of the mixture of cis-isomer and transisomer.
cis-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol[ No CAS ]
trans-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
0.6 g; 1.2 g
With potassium carbonate; In N,N-dimethyl-formamide; at 20℃;Inert atmosphere;
Step 5: synthesis of cis-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol A mixture of <strong>[233764-32-4]4-amino-1-methylcyclohexanol</strong> (2.9 g, 22.3 mmol), 4-chloro-1-fluoro-2-nitro-benzene (3.9 g, 22.3 mmol) and K2CO3 (9.2 g, 66.9 mmol) in DMF (40 mL) was stirred under argon at RT overnight. The resulting mixture was diluted with EA (200 mL) and then washed by saturated NH4Cl solution. The resulting organic layer was concentrated in vacuo. The residue was purified by column chromatography on silica gel (EA:PE=1:19 to 1:4) to afford 0.6 g of cis-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol, 1.2 g of trans-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol, and 3.2 g of the mixture of cis-isomer and trans-isomer.
cis-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol[ No CAS ]
trans-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol[ No CAS ]
4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
0.6 g; 1.2 g; 3.2 g
With potassium carbonate; In N,N-dimethyl-formamide; at 20℃;Inert atmosphere;
A mixture of <strong>[233764-32-4]4-amino-1-methylcyclohexanol</strong> (2.9 g, 22.3 mmol), 4-chloro-1-fluoro-2-nitro-benzene (3.9 g, 22.3 mmol) and K2CO3 (9.2 g, 66.9 mmol) in DMF (40 mL) was stirred under argon at RT overnight. The resulting mixture was diluted with EA (200 mL) and then washed by saturated NH4Cl solution. The resulting organic layer was concentrated in vacuo. The residue was purified by column chromatography on silica gel (EA:PE=1:19 to 1:4) to afford 0.6 g of cis-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol, 1.2 g of trans-4-[(4-chloro-2-nitrophenyl)amino]-1-methylcyclohexanol, and 3.2 g of the mixture of cis-isomer and trans-isomer.
4-bromo-N-(4-chloro-2-nitrophenyl)naphthalene-1-sulfonamide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
90%
With potassium carbonate; In N,N-dimethyl-formamide; at 140.0℃; for 0.23333299999999998h;Microwave irradiation;
Add 1 mmol of 4-bromo-1-naphthalenesulfonamide and 1.1 mmol of 2-nitro-4-chlorofluorobenzene to a reaction tube containing 1.5 mmol of anhydrous potassium carbonate and 5 mL of N,N-dimethylformamide (DMF) Medium, then cover the reaction tube cover,After microwave irradiation for 14 minutes at 140 C, it was cooled to room temperature, opened and acidified. The organic phase was extracted with ethyl acetate and dried over anhydrous sodium sulfate.The filtrate was dehydrated under reduced pressure and column chromatography.The eluent is petroleum ether and acetone. Made a yellow solid,Yield: 90%;
With potassium carbonate; In N,N-dimethyl-formamide; at 140.0℃; for 0.2h;Microwave irradiation;
General procedure: A mixture of benzenesulfonamides (1, 1.0 mmol), halogenated nitrobenzene(2, 1.0 mmol) and K2CO3 (1.1 mmol) were dissolved in DMF in a microwave tube. Then, the reaction mixture was irradiated in a microwave apparatus at 140 C for 12 minutes. After the reaction mixture was cooled to ambient temperature, the product was concentrated, and the crude mixture was purified by column chromatography on silica gel to the desired products 3.
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