(+/-)-4-[4-(diMethylaMino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-(hydroxyMethyl)-benzonitrile, oxalate synthesis
- Product Name:(+/-)-4-[4-(diMethylaMino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-(hydroxyMethyl)-benzonitrile, oxalate
- CAS Number:717133-32-9
- Molecular formula:C22H25FN2O6
- Molecular Weight:432.45
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