Claims
- 1. A process for preparing diorgano telluride compounds under an inert atmosphere comprising the steps of:
- (a) adding an alkali metal to a solution of tetrahydrofuran and naphthalene to form a reducing mixture; said alkali metal selected from the group consisting of lithium, sodium and potassium;
- (b) adding tellurium to said reducing mixture and refluxing to form an alkali metal telluride;
- (c) separating said alkali metal telluride from said reducing mixture;
- (d) combining said alkali metal telluride with a suitable solvent to form a reaction mixture and cooling said reaction mixture to a temperature sufficient to prevent an uncontrolled exothermic reaction upon addition of an organo halide;
- (e) adding an organo halide to said reaction mixture to form a diorgano telluride;
- (f) separating a solid fraction of said reaction mixture from a liquid fraction thereof containing a liquid product;
- (g) extracting said separated solid fraction with said suitable solvent and combining an extract with said liquid fraction;
- (h) removing said solvent by distilling said liquid under an inert gas, leaving a crude product; and
- (i) recovering a diorgano telluride from said crude product by vacuum distillation.
- 2. The process of claim 1 wherein said refluxing step is carried out for at least 8 hours.
- 3. The process of claim 1 wherein said suitable solvent is selected from the group consisting of alcohols having from 1 to 5 carbon atoms, mixtures of said alcohols, mixed solvent systems comprising tetrahydrofuran and one or more of said alcohols, and mixtures of tetrahydrofuran and water.
- 4. The process of claim 1 wherein said temperature sufficient to prevent uncontrolled exothermic reaction upon addition of said organo halide to said alkali metal telluride mixture is from about 0.degree. C. to about -78.degree. C.
- 5. The process of claim 1 wherein said organo halide has the formula RX in which R is an alkyl selected from the group consisting of allyl, methyl, ethyl, n-propyl, iso-propyl, n-butyl, tertiary butyl, and neopentyl; and X is a halide selected from the group consisting of chlorine, bromine and iodine.
- 6. The process of claim 1 wherein said vacuum distillation pressure is at a vacuum from about 2 torr to about 15 torr and a temperature of about 70.degree. C. to about 80.degree. C.
- 7. The process of claim 1 wherein said inert gas is selected from the group consisting of argon and nitrogen.
- 8. A process for preparing diorgano telluride compounds from alkali metal tellurides under an inert atmosphere, said method comprising the steps of:
- (a) combining an alkali metal telluride with a suitable solvent to form a reaction mixture and cooling said reaction mixture to a temperature sufficient to prevent uncontrolled exothermic reaction upon addition of an organo halide, said alkali metal telluride selected from the group consisting of Li2Te, Na2Te and K2Te;
- (b) adding an organo halide to said reaction mixture, said organo halide having the formula RX in which R is an alkyl substituent selected from the group consisting of allyl, methyl, ethyl, n-propyl, iso-propyl, n-butyl, tertiary butyl, and neopentyl; and X is a halide substituent selected from the group consisting of chlorine, bromine and iodine; and
- (c) separating a solid fraction of said reaction mixture from a liquid fraction thereof containing a liquid product;
- (d) extracting said separated solid fraction with said suitable solvent and combining an extract with said liquid fraction;
- (e) removing said solvent by distilling said liquid under an inert gas, leaving a crude product; and
- (f) recovering a diorgano telluride from said crude product by vacuum distillation.
- 9. The process of claim 8 wherein said suitable solvent is selected from the group consisting of alcohols having from 1 to 5 carbon atoms, mixtures of said alcohols, mixed solvent systems comprising tetrahydrofuran and one or more of said alcohols, and mixtures of tetrahydrofuran and water.
- 10. The process of claim 8 wherein said temperature sufficient to prevent uncontrolled exothermic reaction upon addition of said organo halide to said alkali metal telluride is from about 0.degree. C. to about -78.degree. C.
- 11. The process of claim 8 wherein said inert gas is selected from the group consisting of argon and nitrogen.
- 12. The process of claim 8 wherein said vacuum distillation pressure is at a vacuum of about 3 torrs to about 15 torrs and a temperature of about 70.degree. C. to about 80.degree. C.
Parent Case Info
This is a divisional of application Ser. No. 07/066,442 filed on June 26, 1987, now U.S. Pat. No. 5,043,476.
Foreign Referenced Citations (1)
Number |
Date |
Country |
0243495 |
Mar 1987 |
DEX |
Non-Patent Literature Citations (2)
Entry |
Shenai-Khatkhate et al., Journal of Crystal Growth, vol. 77, No. 1-3, pp. -31 (1986). |
Tellurium, W. Charles Cooper Ed., pp. 187-195, Van Nostrand Reinhold Co., New York (1971). |
Divisions (1)
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Number |
Date |
Country |
Parent |
66442 |
Jun 1987 |
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