- Purification of 1-Propanol
-
The main impurities in (CAS NO. ) are usually and 2-propen- l-ol, reflecting the commercial production by hydration of propene. Water can be removed by azeotropic distn either directly (azeotrope contains 28% water) or by using a ternary system, e.g. by adding benzene. Alternatively, for gross amounts of water, refluxing over CaO for several hours is suitable, followed by distn and a further drying. To obtain more nearly anhydrous alcohol, suitable drying agents are firstly NaOH, CaSO4 or K2CO3, then CaH2, aluminium amalgam, magnesium activated with iodine, or a small amount of sodium. Alternatively, the alcohol can be refluxed with n-propylsuccinate or phthalate in a method similar to the one described under EtOH. Allyl alcohol is removed by adding bromine (15mL/L) and then fractionally distilling from a small amount of K2CO3. Propionaldehyde, also formed in the bromination, is removed as the 2,4-dinitrophenylhydrazone. 1-Propanol can be dried down to 20ppm of water by passage through a column of pre-dried molecular sieves (type 3 or 4A, heated for 3h at 300 °C) in a current of nitrogen. Distn from sulfanilic or tartaric acids removes impurities. Albrecht obtained spectroscopically pure material by heating with charcoal to 50-60 °C, filtering and adding 2,4-dinitrophenylhydrazine and a few drops of conc H2SO4. After standing for several hours, the mixture was cooled to 0 °C, filtered and vac distd. and Satchell heated 1-Propanol with 3-nitrophthalic anhydride at 76-110 °C for 15h, then recrystd the resulting ester from H2O, benzene/pet ether (b 100-120 °C)(3:1), and benzene. The ester was hydrolysed under reflux with aq 7.5M NaOH for 45min under nitrogen, followed by distn (also under nitrogen). The fraction (b 87-92 °C) was dried with K2CO3 and stirred under reduced pressure in the dark over 2,4-dinitrophenylhydrazine, then freshly distilled.
Prev:No record
Next:No record - 【Back】【Close 】【Print】【Add to favorite 】
-
Health and Chemical more >
-
Hot Products
- 98-80-6 Phenylboronic acid
- 5921-80-2 Butane, 1,1-dibutoxy-
- 13951-70-7 16alpha-Hydroxyprednisolone
- 844683-65-4 3,3',4-Trifluorobenzhydrol
- 68411-07-4 Lead, copper resorcylate, salicylate
- 10094-45-8 (Z)-N-octadecyldocos-13-enamide
- 481066-70-0 Hydroxyl- and 4-sulfophenyl-modified carbon black. sodium salts
- 97240-79-4 Topiramate
- 482-44-0 Imperatorin
- 89972-79-2 4‘-(4-hydroxyphenyl)-2, 2':6‘, 2“-terpyridine
- 25704-81-8 Anthra[9,1,2-cde]benzo[rst]pentaphene-5,10-dione,dibromo-16,17-dimethoxy-
- 3296-90-0 2,2-Bis(bromomethyl)propane-1,3-diol


