4-氨基苯基三甲基硅烷

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: The synthesis method of compound A-08 is similar to example 9. Just R1 and R3 of Scheme 2 are, respectively, F and p-SiMe3. namely: compound 6 is 4-trimethylsilyl aniline (compound 6a 35 mg); compound 10 is 4-(3-fluoro-pyridine-2-yl)benzoic acid (compound 10c); compound 12 is compound A-08 (62 mg, yield 80.23%). The synthesis method of compound A-08

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

实验步骤: Compound A-04 can be synthesized according to method 2. Just R1 and R3 of Scheme 2 are, respectively, CF3 and p-SiMe3. namely: compound 6 is 4-trimethylsilyl aniline (compound 6a 35 mg); compound 10 is 4-(3-trifluoromethylpyridine-2-yl)benzoic acid (compound 10b); compound 12 is compound A-04 (60 mg, yield 68.3%). Compound A-04 can be synthesized

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

实验步骤: 2.5 g of 12,12-difluorododec-11-enoic acid methyl ester are added at room temperature to 1.53 g of 4-trimethylsilylaniline in 25 ml of toluene. The mixture is stirred for 2 hours at 80° and then concentrated by evaporation in vacuo. The residue is taken up in toluene, the toluene phase is washed with water, dried over sodium sulfate and concentrated to dryness by evaporation. The residue is taken up in hexane:ethyl acetate (9:1) and filtered over silica gel. Evaporation of the filtrate yields the title compound (nD24 =1.5038; compound no. 1-2). concentrated by evaporation in vacuo the toluene phase is washed with water dried over sodium sulfate concentrated to dryness by evaporation filtered over silica gel Evaporation of the filtrate

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

实验步骤: With cooling at 10°, 1.0 g of 6,6-difluorohex-5-enoic acid chloride is added to 1.0 g of 4-trimethylsilylaniline, 0.73 g of trithylamine and 10 mg of 4-N-pyrrolidinopyridine in 25 ml of tetrahydrofuran. The mixture is stirred for 2 hours at room temperature and then concentrated by evaporation in vacuo. The residue is taken up in toluene, the toluene phase is washed with water, dried over sodium sulfate and concentrated to dryness by evaporation. The residue is taken up in hexane:ethyl acetate (9:1) and filtered over silica gel. Evaporation of the filtrate yields the title compound having a melting point of 50°-51° (compound no. 1-1). With cooling at 10° concentrated by evaporation in vacuo the toluene phase is washed with water dried over sodium sulfate concentrated to dryness by evaporation filtered over silica gel Evaporation of the filtrate

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

实验步骤: With cooling at 10°, 1.0 g of 6,6-difluorohex-5-enoic acid chloride is added to 1.0 g of 4-trimethylsilylaniline, 0.73 g of trithylamine and 10 mg of 4-N-pyrrolidinopyridine in 25 ml of tetrahydrofuran. The mixture is stirred for 2 hours at room temperature and then concentrated by evaporation in vacuo. The residue is taken up in toluene, the toluene phase is washed with water, dried over sodium sulfate and concentrated to dryness by evaporation. The residue is taken up in hexane:ethyl acetate (9:1) and filtered over silica gel. Evaporation of the filtrate yields the title compound having a melting point of 50°-51° (compound no. 1-1). With cooling at 10° concentrated by evaporation in vacuo the toluene phase is washed with water dried over sodium sulfate concentrated to dryness by evaporation filtered over silica gel Evaporation of the filtrate

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

实验步骤: The synthesis method of compound A-08 is similar to example 9. Just R1 and R3 of Scheme 2 are, respectively, F and p-SiMe3. namely: compound 6 is 4-trimethylsilyl aniline (compound 6a 35 mg); compound 10 is 4-(3-fluoro-pyridine-2-yl)benzoic acid (compound 10c); compound 12 is compound A-08 (62 mg, yield 80.23%). The synthesis method of compound A-08

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

实验步骤: The synthesis method of compound A-08 is similar to example 9. Just R1 and R3 of Scheme 2 are, respectively, F and p-SiMe3. namely: compound 6 is 4-trimethylsilyl aniline (compound 6a 35 mg); compound 10 is 4-(3-fluoro-pyridine-2-yl)benzoic acid (compound 10c); compound 12 is compound A-08 (62 mg, yield 80.23%). The synthesis method of compound A-08

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

实验步骤: Compound A-04 can be synthesized according to method 2. Just R1 and R3 of Scheme 2 are, respectively, CF3 and p-SiMe3. namely: compound 6 is 4-trimethylsilyl aniline (compound 6a 35 mg); compound 10 is 4-(3-trifluoromethylpyridine-2-yl)benzoic acid (compound 10b); compound 12 is compound A-04 (60 mg, yield 68.3%). Compound A-04 can be synthesized

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 6.0 g of 2,6-difluorobenzoylisocyanate in 20 ml of toluene was added dropwise at room temperature to a mixture of 5.4 g of 4-trimethylsilylaniline, 50 ml of toluene and 100 mg of Dabco®. The reaction mixture obtained was subsequently stirred at 60° C. for 3 hours. The reaction mixture was concentrated by evaporation, and the residue was recrystallised from acetone to obtain 1-(4-trimethylsilylphenyl)-3-(2,6-difluorobenzoyl)-urea of the formula ##STR8## as a white powder having a melting point of 187°-189° C. The reaction mixture obtained The reaction mixture was concentrated by evaporation the residue was recrystallised from acetone

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 6.0 g of 2,6-difluorobenzoylisocyanate in 20 ml of toluene was added dropwise at room temperature to a mixture of 5.4 g of 4-trimethylsilylaniline, 50 ml of toluene and 100 mg of Dabco®. The reaction mixture obtained was subsequently stirred at 60° C. for 3 hours. The reaction mixture was concentrated by evaporation, and the residue was recrystallised from acetone to obtain 1-(4-trimethylsilylphenyl)-3-(2,6-difluorobenzoyl)-urea of the formula ##STR8## as a white powder having a melting point of 187°-189° C. The reaction mixture obtained The reaction mixture was concentrated by evaporation the residue was recrystallised from acetone

反应条件: temp:0.00; pressure:0.00; stir: