تفاعل #53468

معادلة التفاعل

1-amino-4-methylpiperazine

1-[bis(4-chlorophenyl)methyl]-3-{(methylsulfonyl)[3-(pentafluorophenoxycarbonyl)phenyl]methylene]azetidine

ethyl acetate

→

1-[bis(4-chlorophenyl)methyl]-3-{(methylsulfonyl)[(N-4-methylpiperazinylcarbamoyl)phenyl]methylene}azetidine

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   غسيلThe organic phase is washed with 4 times 20 cm3 of water
2. 2
   تجفيفdried over magnesium sulfate
3. 3
   تركيزconcentrated to dryness under reduced pressure (2.7 kPa)
4. 4
   أخرىThe residue is triturated with 10 cm3 of ethyl ether
5. 5
   ترشيحfiltered
6. 6
   أخرىdried

الإجراء التجريبي

0.083 g of 1-amino-4-methylpiperazine is added to a solution of 0.45 g of 1-[bis(4-chlorophenyl)methyl]-3-{(methylsulfonyl)[3-(pentafluorophenoxycarbonyl)phenyl]methylene]azetidine in 5 cm3 of dimethylformamide. The mixture is stirred for 20 hours at room temperature and then 40 cm3 of ethyl acetate are added. The organic phase is washed with 4 times 20 cm3 of water, dried over magnesium sulfate and concentrated to dryness under reduced pressure (2.7 kPa). The residue is triturated with 10 cm3 of ethyl ether, filtered and then dried. 0.2 g of 1-[bis(4-chlorophenyl)methyl]-3-{(methylsulfonyl)[(N-4-methylpiperazinylcarbamoyl)phenyl]methylene}azetidine is obtained in the form of a yellow solid melting at 162° C. [NMR spectrum in DMSO-d6, T=300K, δ in ppm (300 MHz): 2.20 (3H, s, NCH3), 2.40 (4H, m, 2 NCH2), 2.90 (4H, m, 2 NCH2), 2.95 (3H, s, SCH3), 3.80 (2H, s, NCH2), 4.20 (2H, s, NCH2), 4.80 (1H, s, NCH), 7.40 (4H, d, J=7 Hz, 4CH arom.), 7.50 (4H, d, J=7 Hz, 4CH arom.), 7.55 (2H, m, 2CH arom.), 7.80 (2H, m, 2CH arom.), 9.50 (1H, s, CONH)].

المصدر