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Process for preparation of hexafluoroacetone monohydrate

A technology of hexafluoroacetone hydrate and hexafluoroacetone is applied in the preparation of organic compounds, the preparation of hydroxyl compounds, the separation/purification of carbonyl compounds, etc., and can solve the problems of difficult operation, difficult to obtain, unstable compounds and the like

Inactive Publication Date: 2012-05-23
CENT GLASS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Hexafluoroacetone monohydrate is a crystal having a geminal diol structure with a melting point of 46° C. It decomposes and disproportionates into hexafluoroacetone and hexafluoroacetone trihydrate while melting (Patent Document 1). Deliquesces immediately due to moisture in the air, making it an unstable compound that is very difficult to handle and difficult to obtain

Method used

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  • Process for preparation of hexafluoroacetone monohydrate
  • Process for preparation of hexafluoroacetone monohydrate
  • Process for preparation of hexafluoroacetone monohydrate

Examples

Experimental program
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Effect test

Embodiment 1

[0071] [embodiment 1] adding water method

[0072] Add 86g (100mL) toluene, 22g (0.1 mol) HFA·3W, slowly introduce 32 g (0.2 mol) of HFA from the gas inlet while cooling the outside, after introducing a predetermined amount, confirm that the temperature of the reaction solution is below room temperature, then stop the reaction, and obtain 139 g of HFA with a specific gravity of 1.05 Colorless transparent solution (98% yield).

[0073] By NMR ( 13 C, H, F) and F T-IR measurements confirmed the presence of only hexafluoroacetone monohydrate (1,1,1,3,3,3-hexafluoropropane-2-diol) in toluene, and then Karl · The moisture was measured by a Fisher moisture meter, and the molar ratio of hexafluoroacetone and water was confirmed to be 1:1. It should be noted that the water content measurement condition of the Karl Fischer method is to measure water quantitatively produced from hexafluoroacetone monohydrate (1,1,1,3,3,3-hexafluoropropane-2-diol).

[0074] 13 The graph of C-NMR spe...

Embodiment 2

[0075] [embodiment 2] adding water method

[0076] Hexafluoroacetone monohydrate was produced in the same manner as in Example 1 except that 72.5 g of isopropyl ether was used instead of toluene. After the reaction was finished, 127 g of a colorless and transparent solution with a specific gravity of 1.00 was obtained (yield 100%).

[0077] By NMR ( 13 C, H, F) and F T-IR measurements confirmed the presence of only hexafluoroacetone monohydrate (1,1,1,3,3,3-hexafluoropropane-2-diol) in isopropyl ether, In addition, moisture was measured with a Karl Fischer moisture meter, and it was confirmed that the molar ratio of hexafluoroacetone and water was 1:1.

Embodiment 3

[0078] [Example 3] dehydration method

[0079]22 g (0.1 mol) of HFA·3W and 38 g (0.49 mol) of benzene were charged into a 100 mL eggplant-shaped flask equipped with a glass reflux distillation column and a 20 cm distillation column (empty column), and heated in an oil bath while stirring with a stir bar. An azeotropic composition of water / benzene (cloudy at the time of condensation) was distilled at 69°C to 71°C, and the distillation was temporarily stopped when the distillation temperature at the top of the column rose to 73°C. The distilled liquid was separated into two layers, the upper layer was a benzene layer, and the lower layer was a water layer (benzene layer: 6.8 g, specific gravity 0.87, water layer: 3.6 g, specific gravity 1.15). Since the specific gravity of the water layer is larger than 1, it can be seen that a little HFA component is mixed therein. If the distillation is further continued, a new azeotropic composition will distill out at 73.8°C to 74.0°C. The...

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Abstract

Disclosed is a process for the preparation of hexafluoroacetone monohydrate by (1) a hydration method of making hexafluoroacetone absorbed into either water or a hexafluoroacetone hydrate in an organic solvent or (2) a dehydration method of distilling a mixture of a hexafluoroacetone hydrate with an organic solvent to thereby remove a mixture of water and the organic solvent as a low-boiling composition in a simple manner and in a high yield, and thus obtaining a mixture of hexafluoroacetone monohydrate with the organic solvent as a high-boiling composition.

Description

technical field [0001] The present invention relates to the method for producing hexafluoroacetone monohydrate (1,1,1,3,3,3-hexafluoropropane-2-diol), in more detail, relates to the treatment of hexafluoroacetone in the presence of an organic solvent Acetone hydrate dehydration method. Background technique [0002] Hexafluoroacetone is an important compound as a pharmaceutical intermediate or a reaction raw material. Hexafluoroacetone is industrially produced by a method of epoxidizing hexafluoropropylene followed by isomerization, replacing hexachloroacetone obtained by chlorinating acetone with hydrogen fluoride by means of an activated carbon-supported chromium catalyst, etc. Fluorination methods, etc. Since hexafluoroacetone is a gas with a boiling point of -28°C under atmospheric pressure, hexafluoroacetone trihydrate, which can be operated as a composition with a constant boiling point of 106°C, can be used as a raw material in many reactions for convenience in opera...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/82C07C29/00C07C29/82C07C31/42C07C49/167C07C49/173
CPCC07C29/82C07C31/42
Inventor 胜原丰早坂达哉渡边峰男久米孝司
Owner CENT GLASS CO LTD
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