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2-CHLORO-4-METHYLPENTANE synthesis

8synthesis methods
-

Yield:25346-32-1 60%

Reaction Conditions:

with zinc at 50; for 4 h;

Steps:

4

2.534 g of malic acid (0.0189 mol) in solid form, as well as 2.472 g of zinc metal (0.018 mol) in powder form are successively introduced into a 100 mE single-necked flask provided with water-cooled condenser, and 4-methyl-pentan- 2-ol (7 mE) is added in order to disperse the solids and facilitate the stirring of the reaction medium in which the malic acid is partially soluble.The mixture is taken to reflux for 4 hours at 50° C., then it is returned to ambient temperature under stirring for 12 hours until all of the zinc metal has been consumed.12N hydrochloric acid (6 eq.) is then added to the mixture in order to produce ZnC12.Finally, the excess of 4-methyl-pentan-2-ol reacts with the regenerated malic acid in order to produce 2-chloro- 4-methyl-pentane. 15 mE of ether is added to extract the chlorinated derivative. Afier decantation and separation of the aqueous and organic phases, the ether phase is washed twice with 10 mE ofwater then dried over magnesium sulphate. The solution is filtered then concentrated. The crude mixturedistilled (bp=131-134° C.). 60% of 2-chloro-4-methylpen- tane (1.285 g) is isolated pure.

References:

US2015/376224,2015,A1 Location in patent:Paragraph 0758-0763

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