HRID2188493

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID962

Water

H2O

结构：CCCCn1c(=CC=C2CCCC(C=CC3=[N+](CCCC)c4cccc5cccc3c45)=C2c2ccccc2)c2cccc3cccc1c32.F[B-](F)(F)F

HCID75213168

未命名化合物

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

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=C2CCCC(C=CC3=[N+](CCCC)c4cccc5cccc3c45)=C2c2ccccc2)c2cccc3cccc1c32

HCID86664967

未命名化合物

收率 93%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

A mixture of 2.1 g (3 mmol) of 1-butyl-2-(2-{3-[2-(1-butyl-1H-benzo[cd]indol-2-ylidene)ethylidene]-2-phenylcyclohex-1-en-1-yl)ethenyl)-benzo[cd]indol-1-ium tetrafluoroborate, 9.1 g (4.5 mmol) of sodium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate aqueous solution, 20 g of water, and 50 g of methylene chloride was stirred overnight at room temperature, whereupon the organic layer was taken out. The organic layer was washed with water, concentrated in vacuum, combined with methyl isobutyl ketone, and concentrated in vacuum again. 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-phenylcyclohex-1-en-1-yl)ethenyl)-benzo[cd]indol-1-ium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)-propanesulfonate. Brown crystal, 2.6 g, yield 93%.

WORKUP

后处理

washThe organic layer was washed with water
concentrationconcentrated in vacuum
concentrationconcentrated in vacuum again
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-89ed7284dcf14b3d81ab169eaf9cb50c
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

F[B-](F)(F)F.[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[CH2:29][CH2:28][CH2:27][C:26](=[CH:30][CH:31]=[C:32]3[C:40]4[CH:41]=[CH:42][CH:43]=[C:38]5[C:39]=4[C:34](=[CH:35][CH:36]=[CH:37]5)[N:33]3[CH2:44][CH2:45][CH2:46][CH3:47])[C:25]=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:54][C:55]([F:72])([S:68]([O-:71])(=[O:70])=[O:69])[CH:56]([O:61][C:62](=[O:67])[C:63]([CH3:66])([CH3:65])[CH3:64])[C:57]([F:60])([F:59])[F:58].[Na+].O>C(Cl)Cl>[F:72][C:55]([F:54])([S:68]([O-:71])(=[O:69])=[O:70])[CH:56]([O:61][C:62](=[O:67])[C:63]([CH3:65])([CH3:66])[CH3:64])[C:57]([F:58])([F:60])[F:59].[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[CH2:29][CH2:28][CH2:27][C:26](=[CH:30][CH:31]=[C:32]3[C:40]4[CH:41]=[CH:42][CH:43]=[C:38]5[C:39]=4[C:34](=[CH:35][CH:36]=[CH:37]5)[N:33]3[CH2:44][CH2:45][CH2:46][CH3:47])[C:25]=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]