(E)-1,1,1-trichloro-4-ethoxy-3-methylbut-3-en-2-one synthesis

2synthesis methods

Product Name:(E)-1,1,1-trichloro-4-ethoxy-3-methylbut-3-en-2-one
CAS Number:121781-57-5
Molecular formula:C7H9Cl3O2
Molecular Weight:231.5042

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(E)-1,1,1-trichloro-4-ethoxy-3-methylbut-3-en-2-one

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Yield:121781-57-5 100%

Reaction Conditions:

with pyridine in dichloromethane at -10 - 25; for 16 h;

Steps:

D2.2; D3.1

A mixture of (E) -1-ethoxyprop-l-ene (5.00 g, 58.05 ?unol) in pyridine (4.685 ml, 58.05 mmol) was added to at -10⁰C stirring solution of 2, 2, 2-trichloroacetyl chloride (10.56 g, 58.05 mmol) in DCM (15 mL) at a rate of 6-10 drops/minute. After the addition was complete, the mixture was stirred at room temperature for 16 hours. The resulting precipitate was filtered and washed with DCM. The filtrate was concentrated to a residue with a bath temperature of 50⁰C and the residue was dried on high vacuum overnight to give (E) -1, 1, l-trichloro-4- ethoxy-3-methylbut-3-en-2-one (16.14 g, 120% yield). The crude material is used directly in the next step without further purification.

References:

WO2008/11131,2008,A2 Location in patent:Page/Page column 224-225

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References