SU493479A1 - The method of obtaining bis- (1,1 "-diethylferrocenyl) methane - Google Patents

Description

3

102 g of aluminum chloride are added in portions. After 4-5 hours of stirring at room temperature, the reaction mixture is treated with ice and water and stirring is continued for another 30 minutes. The organic part is extracted from the mixture with ether, the aqueous layer is washed several times with ether. The ether extracts are combined and dried with anhydrous magnesium sulphate. The solvent is removed by distillation, unreacted 1,1 diethyl ferrocene is recovered by distillation under reduced pressure. The residue is the product of bis- (1,1-diethylferrocep1 l) - methay.

Yield 24%. d20 1.2183; At 1.5850.

Calculated,%: C, 70.16; H 7.26; Fe 22.60.

Found,%: C 70.38, 70.41; H 7.51; 7.55; Fe 22.42; 22.44.

Example 2. In a three-necked flask equipped with a stirrer and reflux condenser, iomesh, ayut 605 g (2.5 mol) of 1,1-diethylferrocene 85 g (1 mol) of dry methylene chloride. While stirring in an ice bath, 103.5 g of aluminum chloride was added in small portions. After 4-5 hours of stirring at room temperature, the reaction mixture is treated with ice water and stirring is continued for a further 30 minutes. The organic mixture is extracted from the mixture with ether, the aqueous layer is washed several times with ether. The ether extracts are combined and dried with anhydrous magnesium sulphate. The solvent was removed by distillation, and unreacted 1,1-diethylferrocene was returned by distillation under reduced pressure. The residue is the product of bis- (1,1 diethylferroceyl) methane. Yield 14%; dzo 1,2162; pd 1.5826.

Calculated,%: C, 70.16; H 7.26; Fe 22.60.

Paydeno,%: C, 70.52; 70.46; H 7.66; 7.56; Fe 22.25; 22.32.

Example 3. In a four-necked flask equipped with a mechanical stirrer and a reflux condenser, stir, 605 g (2.5 mol) of 1,1-diethylferrocene. When mixing

four

In an ice bath, at the same time, 30 g of naraform (taken as a proportion of 1 formaldehyde in it) and 63.6 g of aluminum chloride are added in small portions. The reaction is continued after P1) by adding the total amount of paraform and aluminum chloride for 3.5-4 hours at room temperature, after which the reaction mixture is treated with ice water and the stirring is continued for more than 30 minutes. The organic portion is extracted from the reaction mixture with ether, the ether extracts are combined and dried with anhydrous magnesium sulfate. The solvent was removed by distillation, and unreacted 1,1-diethylferrocene was returned by distillation under reduced pressure. The residue is the product of bis- (1,1-diethylferrocenl) methane. Yield 40%; dw 1.2293;

By 1.6804.

Calculated,%: C, 70.16; П 7.26; Fe 22.60.

Found,%: C, 70.46; 70.54; P 7.54; 7.59; Fe 22.21; 22.40.

Subject invention

Claims (4)

1. A process for the preparation of bis (l, l-diethylfeprocenyl) methane, characterized in that 1,1-diethyl ferrocene is subjected to condensation with a formaldehyde derivative or methylene chloride in the presence of anhydrous aluminum chloride, followed by isolation of the target product by known methods. 2. A method according to claim 1, characterized in that paraform or dimethylformal is used as a formaldehyde derivative. 3.Ciose on pi. 1 and 2, characterized in that 1,1-diethyl ferrocene and condensing ageit are used in a molar ratio of 2.5-1, respectively. 4. Ways on. 1, 2 and 3, characterized in that anhydrous aluminum chloride is taken in an amount of 10-15% by weight of the reactants.