HRID2188492

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID962

Water

H2O

结构：CC(C)(C)C(=O)OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-].[Na+]

HCID86616368

未命名化合物

结构：CCCCn1c(=CC=C2CCC(C=CC3=[N+](CCCC)c4cccc5cccc3c45)=C2N(c2ccccc2)c2ccccc2)c2cccc3cccc1c32.[O-][Cl+3]([O-])([O-])[O-]

HCID86664966

未命名化合物

PRODUCTS

生成物

结构：CC(C)(C)C(=O)OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-].CCCCn1c(=CC=C2CCC(C=CC3=[N+](CCCC)c4cccc5cccc3c45)=C2N(c2ccccc2)c2ccccc2)c2cccc3cccc1c32

HCID86664965

未命名化合物

收率 86%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID7909

4-Methyl-2-pentanone

C6H12O

PROCEDURE

实验过程

A mixture of 0.80 g (1 mmol) of 1-butyl-2-(2-{3-[2-(1-butyl-1H-benzo[cd]indol-2-ylidene)ethylidene]-2-(N,N-diphenylamino)cyclopent-1-en-1-yl)ethenyl)-benzo[cd]indol-1-ium perchlorate, 3.1 g (1.5 mmol) of sodium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate aqueous solution, 16 g of water, and 16 g of methyl isobutyl ketone was stirred overnight at room temperature, whereupon the organic layer was taken out. The organic layer was washed with water and concentrated in vacuum. Diisopropyl ether was added to the residue for recrystallization. The crystal was collected and dried in vacuum, obtaining the target compound, 1-butyl-2-(2-{3-[2-(1-butyl-1H-benzo[cd]indol-2-ylidene)ethylidene]-2-(N,N-diphenylamino)cyclopent-1-en-1-yl)ethenyl)-benzo[cd]-indol-1-ium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propane-sulfonate. Brown crystal, 0.88 g, yield 86%.

WORKUP

后处理

washThe organic layer was washed with water
concentrationconcentrated in vacuum
additionDiisopropyl ether was added to the residue for recrystallization
customThe crystal was collected
customdried in vacuum

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-d7f5915dabd7442ea59fcfd7e9868533
来源数据集: uspto-grants-2012_12
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08323536B2
来源说明: uspto-grants-2012_12

反应 SMILES

Cl([O-])(=O)(=O)=O.[CH2:6]([N+:10]1[C:18]2[C:13]3[C:14](=[CH:19][CH:20]=[CH:21][C:12]=3[C:11]=1[CH:22]=[CH:23][C:24]1[CH2:28][CH2:27][C:26](=[CH:29][CH:30]=[C:31]3[C:39]4[CH:40]=[CH:41][CH:42]=[C:37]5[C:38]=4[C:33](=[CH:34][CH:35]=[CH:36]5)[N:32]3[CH2:43][CH2:44][CH2:45][CH3:46])[C:25]=1[N:47]([C:54]1[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=1)[C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1)[CH:15]=[CH:16][CH:17]=2)[CH2:7][CH2:8][CH3:9].[F:60][C:61]([F:78])([S:74]([O-:77])(=[O:76])=[O:75])[CH:62]([O:67][C:68](=[O:73])[C:69]([CH3:72])([CH3:71])[CH3:70])[C:63]([F:66])([F:65])[F:64].[Na+].O>C(C(C)=O)C(C)C>[F:78][C:61]([F:60])([S:74]([O-:77])(=[O:75])=[O:76])[CH:62]([O:67][C:68](=[O:73])[C:69]([CH3:71])([CH3:72])[CH3:70])[C:63]([F:64])([F:66])[F:65].[CH2:6]([N+:10]1[C:18]2[C:13]3[C:14](=[CH:19][CH:20]=[CH:21][C:12]=3[C:11]=1[CH:22]=[CH:23][C:24]1[CH2:28][CH2:27][C:26](=[CH:29][CH:30]=[C:31]3[C:39]4[CH:40]=[CH:41][CH:42]=[C:37]5[C:38]=4[C:33](=[CH:34][CH:35]=[CH:36]5)[N:32]3[CH2:43][CH2:44][CH2:45][CH3:46])[C:25]=1[N:47]([C:54]1[CH:55]=[CH:56][CH:57]=[CH:58][CH:59]=1)[C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1)[CH:15]=[CH:16][CH:17]=2)[CH2:7][CH2:8][CH3:9]