ChemicalBook CAS DataBase List Di-tert-butylchlorophosphane

Di-tert-butylchlorophosphane synthesis

7synthesis methods

Product Name:Di-tert-butylchlorophosphane
CAS Number:13716-10-4
Molecular formula:C8H18ClP
Molecular Weight:180.66

819-19-2

13716-10-4

General procedure for the synthesis of di-tert-butylphosphonium chloride from di-tert-butylphosphine: Di-tert-butylphosphine (13.5 g, 92 mmol) was added to a three-necked round-bottomed flask fitted with a thermometer, a charging funnel and a condenser under the protection of nitrogen and heated to 83-84 °C. The synthesis of di-tert-butylphosphonium chloride from di-tert-butylphosphine was carried out by the following procedure. Octyl trichloroacetate (25.4 g, 92 mmol) was slowly added dropwise over a period of 20 minutes. After the dropwise addition, the reaction mixture was continued to be stirred at 70 °C for 20 min, which showed 0.6% unreacted di-tert-butylphosphine by GC analysis. The addition funnel was removed and the short-circuit distillation head was adapted for distillation. Two fractions were collected and the former fraction (1.24 g) was discarded. The second fraction was collected to give 13 g (78.2% yield) of di-tert-butylphosphonium chloride as a clear, colorless liquid with a boiling point of 48-52 °C/3.2 mbar (literature value 48 °C/3 mm Hg). The purity of the product was 97% by GC-FID.

819-19-2 Synthesis

819-19-2
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$74.00/1g

13716-10-4
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$22.00/1g

Yield:13716-10-4 78.2%

Reaction Conditions:

with n-octyl trichloroacetate at 70 - 84; for 0.666667 h;Product distribution / selectivity;

Steps:

6

Di-tert-butyl phosphine (13.5 g, 92 mmol) was charged to a three necked round bottomed flask equipped with thermometer, addition funnel and condenser with nitrogen blanket, and heated to 83-84°C. Octyl trichloroacetate (25.4 g, 92 mmol) was added dropwise over a period of 20 min. After completion of the addition, the resultant reaction mixture was digested for an additional 20 min at 70⁰C, after which time it was analysed by GC indicating the presence of 0.6% unreacted di- tert-butylphosphine .The addition funnel was removed and the flask was equipped with a short path distillation head. Distillation resulted in two fractions. The fore-cut (1.24 g) was discarded. The second fraction provided 13 g (78.2%) of di-tert- butylchlorophosphine as clear colourless liquid. Boiling point 48-52°C/3.2 mbar (lit. 48°C/3 mmHg) . Purity 97% by GC- FID.

References:

WO2009/147495,2009,A2 Location in patent:Page/Page column 17

507-20-0 Synthesis