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HRID230498

反应详情

EQUATION

反应方程式

HRID 230498 的结构方程式

REACTANTS

反应物

5
结构：NS(=O)(=O)c1cccc(F)c1
HCID150924

3-Fluorobenzenesulfonamide

C6H6FNO2S

结构：O=S(=O)(Cl)c1cccc(F)c1
HCID2734258

3-Fluorobenzenesulfonyl chloride

C6H4ClFO2S

结构：CCOCC.Cl
HCID10953452

未命名化合物

结构：CC(C)(C)OC(=O)N1CCCN(c2ccc(N)c(N)c2)CC1
HCID22272464

1,1-Dimethylethyl 4-(3,4-diaminophenyl)hexahydro-1H-1,4-diazepine-1-carboxylate

C16H26N4O2

结构：CC(C)(C)OC(=O)N1CCCN(c2ccc(NS(=O)(=O)c3cccc(F)c3)c(N)c2)CC1
HCID22272531

未命名化合物

PRODUCTS

生成物

1
结构：Cl.O=S(=O)(Nc1ccc(N2CCCNCC2)cc1NS(=O)(=O)c1cccc(F)c1)c1cccc(F)c1
HCID10209725

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

The compound was prepared from 2-amino-5-(4-t-butyloxycarbonyl-1-homopiperazinyl)aniline and 3-flourobenzenesulfonyl chloride. Purification by column chromatography (CH2Cl2/MeOH/heptane, 4:1:15) gave a mixture of N-{2-amino-4-[4-t-butyloxycarbonyl-homopiperazin-1-yl-]phenyl}3-fluorobenzenesulfonamide and N-{4-[4-t-butyloxycarbonyl]homopiperazinyl)-2-[(3-flourophenylsulfonyl)amino]phenyl}-3-fluorobenzenesulfonamide (0.180 g, 73%). Boc-deprotection was achieved by dissolving the mixture in small amount of MeOH and adding HCl/ether. The mixture was let at r.t. for 0.5 h. Purification by preparative HPLC gave N-(4-(1,4-diazepan-1-yl)-2-{[(3-fluorophenyl)sulfonyl]amino}phenyl)-3-fluorobenzenesulfonamide hydrochloride Anal. (C23H27ClN4O4S2) C, H, N, S.; M+524.4 Calcd 522.12.

WORKUP

后处理

  1. customPurification by column chromatography (CH2Cl2/MeOH/heptane, 4:1:15)
  2. customgave
  3. customPurification by preparative HPLC