Preparation of high purity tetrahydrocarbylammonium tetrahydridoborates
First Claim
1. The process for preparing high purity tetrahydrocarbylammonium tetrahydridoborates of the formula
wherein R1, R2, R3 and R4 may be independently selected from the group consisting of alkyl containing 1-6 carbon atoms, which comprises carrying out the following steps under anhydrous conditions and at temperatures from about 30°
C. up to the boiling point of the reaction mixture;
(a) reacting a tetrahydrocarbylammonium salt starting material of the formula
space="preserve" listing-type="equation">R.sub.1 R.sub.2 R.sub.3 R.sub.4 N.sup.+ X.sup.-wherein R1, R2, R3 and R4 are as defined above and wherein X- is an anion from an inorganic salt, with at least 8% molar excess of an alkali metal hydroxide of the formula
space="preserve" listing-type="equation">MOHwherein M is an alkali metal, in the presence of anhydrous ethanol to produce a tetrahydrocarbylammonium hydroxide of the formula
space="preserve" listing-type="equation">R.sub.1 R.sub.2 R.sub.3 R.sub.4 N.sup.+ OH.sup.-wherein R1, R2, R3 and R4 are as defined above in solution with the ethanol, and the corresponding alkali metal salt,(b) removing the alkali metal salt, and(c) reacting the R1 R2 R3 R4 N+ OH- organic solvent solution with an alkali metal borohydride of the formula
space="preserve" listing-type="equation">M.sub.1 BH.sub.4wherein M1 is an alkali metal.
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Abstract
High purity tetrahydrocarbylammonium tetrahydridoborates are prepared under anhydrous conditions by reacting tetrahydrocarbylammonium salts with at least 8% molar excess of an alkali metal hydroxide in the presence of ethanol to produce the corresponding tetrahydrocarbylammonium hydroxides and alkali metal salts, removing the alkali metal salts and adding an alkali metal borohydride to the solution to produce the corresponding tetrahydrocarbylammonium tetrahydridoborates and alkali metal hydroxides.
29 Citations
13 Claims
- 1. The process for preparing high purity tetrahydrocarbylammonium tetrahydridoborates of the formula
- space="preserve" listing-type="equation">R.sub.1 R.sub.2 R.sub.3 R.sub.4 NBH.sub.4
wherein R1, R2, R3 and R4 may be independently selected from the group consisting of alkyl containing 1-6 carbon atoms, which comprises carrying out the following steps under anhydrous conditions and at temperatures from about 30°
C. up to the boiling point of the reaction mixture;(a) reacting a tetrahydrocarbylammonium salt starting material of the formula
space="preserve" listing-type="equation">R.sub.1 R.sub.2 R.sub.3 R.sub.4 N.sup.+ X.sup.-wherein R1, R2, R3 and R4 are as defined above and wherein X- is an anion from an inorganic salt, with at least 8% molar excess of an alkali metal hydroxide of the formula
space="preserve" listing-type="equation">MOHwherein M is an alkali metal, in the presence of anhydrous ethanol to produce a tetrahydrocarbylammonium hydroxide of the formula
space="preserve" listing-type="equation">R.sub.1 R.sub.2 R.sub.3 R.sub.4 N.sup.+ OH.sup.-wherein R1, R2, R3 and R4 are as defined above in solution with the ethanol, and the corresponding alkali metal salt, (b) removing the alkali metal salt, and (c) reacting the R1 R2 R3 R4 N+ OH- organic solvent solution with an alkali metal borohydride of the formula
space="preserve" listing-type="equation">M.sub.1 BH.sub.4wherein M1 is an alkali metal. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13)
Specification
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- Resources
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Current AssigneeAllied Chemical Corporation (Honeywell International Inc.)
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Original AssigneeAllied Chemical Corporation (Honeywell International Inc.)
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InventorsEvans, Francis E., Robinson, Martin A., Lind, Charles J.
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Primary Examiner(s)Evans, Joseph E.
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Application NumberUS05/951,822Time in Patent Office659 DaysField of Search260/567.6 MUS Class Current564/8CPC Class CodesC07F 5/022 without C-boron linkages
