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6-Bromo-7-methyl-1,4-dioxaspiro[4.4]non-6-ene synthesis

4synthesis methods
80963-36-6 Synthesis
2-BROMO-3-METHYL-2-CYCLOPENTEN-1-ONE

80963-36-6
15 suppliers
$117.00/1g

6-Bromo-7-methyl-1,4-dioxaspiro[4.4]non-6-ene

70156-97-7
8 suppliers
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Yield:70156-97-7 88%

Reaction Conditions:

with toluene-4-sulfonic acid;Triethyl orthoacetate in ethylene glycol at 20; for 3 h;Inert atmosphere;

Steps:

Synthesis of Intermediate K

To a 500 mL rbf, equipped with a stirrer bar, under an atmosphere of Argon was added 200 mL of triethyl orthoacetate (Aldrich), 7.8 g, 40 mmol, of Compound J and 38 mg, 0.2 mmol of para- toluenesulfonic acid. The reaction mixture was stirred at room temperature for 3 hours or until TLC analysis indicates the reaction has gone to completion and the product was distilled off under vacuum to give Compound K as a clear oil which solidified to a white solid on cooling in 88% yield >96% purity

References:

WO2014/145302,2014,A2 Location in patent:Page/Page column 34; 38