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Terbuficin synthesis

2synthesis methods
-

Yield:-

Reaction Conditions:

with sodium hydroxide in methanol;

Steps:

3.a a.

a. Bis(4'-hydroxy-3',5'-di-tert.butyl-phenyl)ethanoic acid A solution of 129 g of dichloracetic acid in 40 g of methanol was added dropwise in portions at 85° C within 6 hours to a suspension of 103 g of 2,6-di-tert.butyl-phenol in 200 g of methanol and 147 g of sodium hydroxide. The mixture was then stirred for about 20 hours at 80° C. After cooling to 20° C, it was acidified with dilute hydrochloric acid (pH 5-6), whereupon the crude bis(4'-hydroxy-3',5'-di-tert.-butylphenyl) ethanoic acid of a yellow orange color precipitated. After drying and subsequent recrystallization from cyclohexane, the pure acid was obtained as a white crystallized compound, m.p. 211° C. Analysis: C30 H44 O4: Found: C, 76.9%; O, 13.5%; H, 9.3%. Calculated: C, 77.0%; O, 13.7%; H, 9.4%.

References:

US4007282,1977,A

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