HRID565755

反应详情

EQUATION

反应方程式

REACTANTS

反应物

$结构：O=C(O)/C=C\C(=O)O$

HCID444266

Maleic acid

C4H4O4

结构：O=S(=O)(CCCCCCN1CCN(C(c2ccccc2)c2cccc(Cl)c2)CC1)NC1CC1

HCID15895709

未命名化合物

PRODUCTS

生成物

$结构：O=C(O)/C=C\C(=O)O.O=C(O)/C=C\C(=O)O.O=S(=O)(CCCCCCN1CCN(C(c2ccccc2)c2cccc(Cl)c2)CC1)NC1CC1$

HCID86756218

未命名化合物

收率 50.3%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

N-Cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide (253 mg, 0.52 mmol) prepared in the same manner as in Example 1 was dissolved in methanol (15 ml). Maleic acid (138 mg, 1.19 mmol) was added thereto. After dissolving the mixture with heating, the solvent was removed by evaporation in vacuo. Acetone-diethyl ether was added to the residue, and the precipitated crystals were collected by filtration. The crystals were recrystallized from ethyl acetate, to give N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide dimaleate (189 mg) as colorless prisms (yield based on N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl)hexanesulfonamide: 50.3%).

WORKUP

后处理

dissolutionAfter dissolving the mixture
temperaturewith heating
customthe solvent was removed by evaporation in vacuo
additionAcetone-diethyl ether was added to the residue
filtrationthe precipitated crystals were collected by filtration
customThe crystals were recrystallized from ethyl acetate
customto give

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-131df067850048a6ac5e768697bd022f
来源数据集: uspto-grants-2001_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US06172228B2
来源说明: uspto-grants-2001_01

反应 SMILES

[CH:1]1([NH:4][S:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH:20]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH2:15]2)(=[O:7])=[O:6])[CH2:3][CH2:2]1.[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]\[C:37]([OH:39])=[O:38]>CO>[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]\[C:37]([OH:39])=[O:38].[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]\[C:37]([OH:39])=[O:38].[CH:1]1([NH:4][S:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH:20]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH2:15]2)(=[O:7])=[O:6])[CH2:3][CH2:2]1