4,4-difluoro-1-(3-fluoro-4-methoxyphenyl)butane-1,3-dione synthesis
- Product Name:4,4-difluoro-1-(3-fluoro-4-methoxyphenyl)butane-1,3-dione
- CAS Number:170570-77-1
- Molecular formula:C11H9F3O3
- Molecular Weight:246.18
Yield:170570-77-1 96%
Reaction Conditions:
with hydrogenchloride;sodium methoxide in tert-butyl methyl ether;
Steps:
2.2 Step 2
Step 2 Preparation of 4,4-difluoro-1-(3-fluoro-4-methoxyphenyl)-butane-1,3-dione Ethyl difluoroacetate (4.06 g, 32.7 mmol) was dissolved in methyl tert-butyl ether (50 mL). To the stirred solution was added 25 weight % sodium methoxide (7.07 g, 32.7 mmol) followed by 3'-fluoro-4'-methoxyacetophenone from Step 1 (5.0 g, 29.7 mmol). After stirring for 16 hours, 1N HCl (50 mL) was added. The organic layer was collected and washed with water (2*50 mL), dried over anhydrous MgSO4, filtered, and added to hexanes to precipitate a tan solid (7.0 g, 96%): mp 70-72° C.
References:
US6376528,2002,B1
321-28-8
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