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ChemicalBook CAS DataBase List (+/-)-4-[4-(diMethylaMino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-(hydroxyMethyl)-benzonitrile, oxalate
717133-32-9

(+/-)-4-[4-(diMethylaMino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-(hydroxyMethyl)-benzonitrile, oxalate synthesis

1synthesis methods
-

Yield:-

Reaction Conditions:

in methanol at 25 - 60; for 3 h;Product distribution / selectivity;

Steps:

1 Preparation of (+-)-4-[4-Dimethylamino)-1-(4-fluorophenyl)-1-Hydroxybutyl]-3-(Hydroxymethyl)-Benzonitrile,

Oxalate [(+-)-Diol Oxalate Salt] (+-)-Diol compound (VI) (12 g, 0.035 mol) and oxalic acid dihydrate (4.64 g, 0.0368, 1.05 mol) were added to methanol (36 ml) and heated the contents to 55-60° C. to obtain a clear solution. The obtained solution was cooled to 25-30° C. and stirred for 3 h to complete the crystallization. Product was filtered and thereafter, dried at 50-60° C. under reduced pressure to yield 11 g of diol oxalate salt (VIa) with HPLC purity 99.93%.

References:

US2009/99375,2009,A1 Location in patent:Page/Page column 4

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