Acetic Add, Glacial

Acetic add (glacial), acetone, butanol, butyl acetate, cyclohexane, dioxane, ethyl Cellosolve, ethylene chloride, methyl acetate, methyl ethyl ketone, methyl isobutyl ketone, toluene... 

Acetylating Mixture. Equal vols. of acetic anhydride and glacial acetic add (p. 107). (A special mixture is used for quantitative acetylation see p. 451.)... 

Spray solution Carefully add 8 ml cone, sulfuric add and 0.5 ml anisaldehyde under cooling with ice to a mixture of 85 ml methanol and 10 ml glacial acetic add [1,4, 8,11,16]. 

In a first step oxidized aromatic amines are reduced with titaniumflll) chloride in glacial acetic add solution and then condensed to a colored Schiff s base with 4-(dimethylamino)-benzaldehyde (cf. Chapter 2). 

TLC plates Silica gel 60 with concentrating zone (Mekck). 1-Propanol - glacial acetic add (90 -i-10). 

Propanol — 0.75% aqueous boric acid — glacial acetic add (40 + 5 + 1). 

Dissolve 0.5 g selenium dioxide in SO ml methanol and add glacial acetic add [2]. 

Hydrolysis urith Hydrogen Bromide in Glacial Acetic Add... 

The normality of the stronger solution is checked once a month in the following way 0.1 ml ethyl hydroperoxide solution +2 ml potassium iodide (20 g/100 ml) + 2 chops of glacial acetic add are placed in a porcelain crucible, covered with a lid, and allowed to stand at room temperature for 4 hours. The amount of iodine released is then titrated with 0.05 N sodium thiosulfate. 

Buffered supporting electrolyte Dissolve 10 g of KN03 and 8.2 g of sodium acetate in 500 ml of DW. Add glacial acetic acid carefully until a pH of 4.2 is achieved (pH Meter) (approximately 10 ml of the acid will be required),... 

Add glacial acetic acid dropwise until the pH is =2.5, and an orange precipitate forms. 

Paludrine in bulk may be estimated by titration with perchloric acid in glacial acetic add 653), or gravimetrically as its copper complex... 

A. (o-Bromo-p-chloroacetophenone oxime. A 500-mL, four-necked, round-bottomed flask equipped with a dropping funnel (closed with a giass stopper), mechanicai stirrer, drying tube (calcium chioride, CaCij), and a thermometer is charged with p-chloroacetophenone (38.6 g, 0.25 moi), glacial acetic add (220 mL) and aqueous hydrobromic acid (HBr) [1 mL, 48 % (w/w). Note 1]. The flask is immersed in a water bath (15°C, Note 2) and bromine (40.0 g, 0.25 mol) is added from the dropping funnei at such a... 

C. 4-Methoxycarbonyl-2-methyl-1,3-oxazole (3). A flame-dried, 50-mL, twonecked, round-bottomed flask is equipped with a stir bar, reflux condenser, rubber septum, and an argon inlet. The flask is charged with glacial acetic add (15 mL) which is heated to reflux. To this is added crude potassium methyl a-[(methoxyethylidene)-amino]-p-... 

If the atophan does not crystallise—this is rarely the case unless pyruvic add which has been standing for some time is employed—pour the reaction mixture into a solution of 25 g. of potassium hydroxide in 1 litre of water, and extract the resulting solution two or three times with ether. Place the ether extracts in the ETHER RESIDUES bottle. Treat the aqueous layer with 70 ml. of glacial acetic add with vigorous stirring. Allow to stand for several hours and collect the crude atophan by filtration with suction. 

Other tetrasnhstituted olefins (Eq. 115) have recently boon reported18 4-1844 to yield the corresponding epoxides on oxidation with chromic noid in glacial acetic add, Mosher and co-workers also noted in addition the formation of significant proportions of cyclic carbonate when all traces of winter were excluded from tfio reaction medium by addition of acetic anhydride.1944... 

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