ChemicalBook CAS DataBase List 2,2,3,3,4,4,4-Heptafluoro-1-butanol

2,2,3,3,4,4,4-Heptafluoro-1-butanol synthesis

11synthesis methods

Product Name:2,2,3,3,4,4,4-Heptafluoro-1-butanol
CAS Number:375-01-9
Molecular formula:C4H3F7O
Molecular Weight:200.05

425-23-0
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375-01-9
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Yield:375-01-9 92%

Reaction Conditions:

with RuCl2(DPPEA)(±DAIPEN);hydrogen;sodium methylate in isopropyl alcohol at 80; under 750.075 - 15001.5 Torr; for 30 h;Autoclave;

Steps:

1
To the autoclave, 128 g of isopropylidene isobutyrate and 128 g of isopropyl alcohol were added, and 35.8 mg of hydrogenation The catalyst (RuCl2 (DPPEA) (± DAIPEN)) and 27 mg of sodium methoxide were sealed and charged with N2 to a pressure of 0.1 MPa for three times, And then the temperature is reduced to 80 ° C, the pressure is increased to 2.0 MPa, the reaction is completed after 30 hours, cooling, the cooled reaction liquid is transferred to the distillation unit, the temperature is raised, and the control reflux ratio 12: 1, collecting the temperature of 82 ~ 88 fractions (distillate is solvent isopropyl alcohol), after the end of the cooling, the remaining liquid into the equal volume of distilled water, stir, With a mass fraction of about 1% hydrochloric acid to adjust the pH value of 7, standing stratification, liquid separation, the lower organic phase with anhydrous sodium sulfate drying, Filtration, filtrate distillation after the fractions weighing 92g, that is, heptafluorobutanol, gas phase detection of 99.3% purity, yield 92%.

References:

Wuhan Institute of Technology;Wuhan Kaisen Chemical Co., Ltd.;Xi, Qiang;Hu, Yang;Feng, Weiwei;Shu, Chang;Yang, Haitao;Zeng, Tianyu;Zhang, Zhipeng CN104829432, 2017, B Location in patent:Paragraph 0024

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