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ChemicalBook CAS DataBase List 4-(Phthalimide)cyclohexanol

4-(Phthalimide)cyclohexanol synthesis

3synthesis methods
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Yield: 79%

Reaction Conditions:

with pyridinium p-toluenesulfonate in N,N-dimethyl-formamide;toluene for 15 - 17 h;Product distribution / selectivity;Heating / reflux;

Steps:

1.A
A) SOOgms (2.608mole) of Trans-4-aminocyclohexanol was dissolve in 1500mlDimethyl formamide and 1500ml of Toluene. Add 386gms(2.608mole) of Phthalicanhydride and 3gm(0.012mole) pyridinium p-toluene sulphonate. The reaction mixtureis refluxed and remove water continuously from water separator, maintain this conditionfor 15-17 hrs. Evaporate solvent under reduced pressure. Add chloroform (3000ml).Wash organic part with 1000ml of 5%NaHCO3, then wash with 1000ml of brine solution.After concentration of reaction mass, crystallize residue in Isopropyl alcohol.YIELD :503gms(79%)PURITY: 99.66%

References:

ALEMBIC LIMITED WO2006/3677, 2006, A1 Location in patent:Page/Page column 10; 15