Sodium Hydroxide → HCID 131733080, compound

Participants

Reaction Steps

A mixture of 1.86 g (2 mmol) of 3-butyl-2-(2-{3-[2-(3-butyl-1,1-dimethyl-1H-benzo[e]indol-2(3H)-ylidene)-ethylidene]-2-(phenylsulfonyl)cyclopent-1-en-1-yl}ethenyl)-1,1-dimethyl-1H-benzo[e]indol-3-ium p-toluenesulfonate, 2.21 g (3 mmol) of a 56% tris(trifluoromethanesulfonyl)methide acid aqueous solution, 0.48 g of a 25% sodium hydroxide aqueous solution, 30 g of water, and 30 g of methyl isobutyl ketone was stirred for 8 hours at room temperature, whereupon the organic layer was taken out. The organic layer was combined with 0.74 g (1 mmol) of a 56% tris(trifluoromethanesulfonyl)methide acid aqueous solution and 30 g of water and stirred overnight, 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, 3-butyl-2-(2-{3-[2-(3-butyl-1,1-dimethyl-1H-benzo[e]indol-2(3H)-ylidene)ethylidene]-2-(phenylsulfonyl)cyclopent-1-en-1-yl}ethenyl)-1,1-dimethyl-1H-benzo[e]indol-3-ium tris(trifluoromethylsulfonyl)methide. Brown crystal, 2.2 g, yield 92%.

Provenance & Evidence