反应 #1797553

反应方程式

compound A8

N-(2-fluoro-4-methyl-phenyl)-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide

7-[2-(6-phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-4,5,6,7-tetrahydro-3H-azepin-2-ylamine

7-[2-(6-Phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-4,5,6,7-tetrahydro-3H-azepin-2-ylamine

compound 1

7-[2-(6-Phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-4,5,6,7-tetrahydro-3H-azepin-2-ylamine

ammonia

N-(2-fluoro-4-methyl-phenyl)-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide

→

pure title compound

4-{2-[2-(7-Amino-3,4,5,6-tetrahydro-2H-azepin-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-N-(2-fluoro-4-methyl-phenyl)-benzenesulfonamide

溶剂

methanol

反应条件

后处理

1. 1
   其他The title compound is synthesized
2. 2
   过滤Subsequently, the mixture is filtered with suction
3. 3
   洗涤The residue is washed with 20 ml of methanol
4. 4
   其他dried under high vacuum

实验过程

The title compound is synthesized as described for 7-[2-(6-phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-4,5,6,7-tetrahydro-3H-azepin-2-ylamine (compound 1) from 100 mg of N-(2-fluoro-4-methyl-phenyl)-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide (compound A8) and 4.30 ml of methanol containing ammonia (strength: 7.0 M) at 50° C. for 90 hours. Subsequently, the mixture is filtered with suction. The residue is washed with 20 ml of methanol and dried under high vacuum to afford 61 mg of the pure title compound as an amorphous, colorless solid of m.p. 265° C. ESI-MS: 521.2 (MH+), TLC: Rf=0.28 (HPTLC RP-C18; acetonitrile/water 2:1 parts by volume).

来源