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ChemicalBook CAS DataBase List 1,3-DICHLORO-1,1-DIFLUOROPROPANE

1,3-DICHLORO-1,1-DIFLUOROPROPANE synthesis

9synthesis methods
-

Yield:677-21-4 91 %Chromat. ,819-00-1 9 %Chromat.

Reaction Conditions:

with hydrogen fluoride;activated by HF amorphous Zn/chromia catalyst at 200;

Steps:

5

Example 5: Hydrofluorination of 250fb (CCbCH2CH2CI) at elevated pressureThe reactor, made from an lnconnel tube 30 cm x 0.5 inches, was charged with 6g of a 5.2 % Zn/Chromia catalyst which was essentially amorphous in character, which was treated as follows:The catalyst was first dried by heating under nitrogen (80 ml/min) at 25O0C and 3 barg for 48 hours. Next, pre-fluorination of the catalyst was begun by introducing HF (4 ml/min) into the nitrogen stream and increasing the temperature to 3000C for 16 hours. During the last 5 hours the nitrogen flow was reduced steadily to zero. The temperature was then ramped to 38O0C at 25°C/hr and held at 38O0C for 7 hours and then cooled to 25O0C at 25°C/hr.A feed mixture comprising 250fb (3 ml/min) and HF (45 ml/min) was then passed over the catalyst at 15 barg and 2000C. The gases exiting the reactor were periodically sampled and analysed by GC after passing through an alkaline scrubber to remove acid gases. The only products detected in the reactor off-gases following following removal of the acid gases were the desired product 1243zf (91 mol %, CF3CH=CH2) and 1 ,1- difluoro-1,3-dichloropropane (9 mol %, CF2CICH2CH2CI).It is believed that the 1 ,1-difluoro-1,3-dichloropropane could be converted to 1243zf by altering the reaction conditions (e.g. by increasing the temperature and/or contact time). In this way, 250fb could be fully converted in 100% selectivity to 1243zf in a single pass.

References:

WO2009/125199,2009,A2 Location in patent:Page/Page column 32

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