Glacial AcOH

Purified by recrystn from glacial AcOH or from C6Hg and the yellow needles are dried in an oven at 100° until the odour of the solvent is absent. It is sparingly soluble in EtOH and Me2CO. [Bogert and Stull Org Synth Coll Vol I 220 7947 Bauer and Cymerman J Chem Soc 3434 7949.]... 

Recrystd twice from glacial AcOH and dried at 100° in a vacuum. 

Bis-(triphenylpbospbine)nickel(II) chloride [14264-16-5] M 654.2, m 225 (dec). Wash with glacial AcOH and dry in vac over H2SO4 and KOH until AcOH is removed. [J Chem Soc 719 1958.]... 

Indium (III) sulfate (5H2O) [17069-79-3] M 607.9, d 3.44. Dissolve in strong H2SO4 and slowly evaporate at ca 50°. Wash crystals with glacial AcOH and then heat in a furnace at a temperature of 450-500° for 6h. Sol in H2O is 5%. The pentahydrate is converted to an anhydrous hygroscopic powder on heating at 500° for 6h but heating above this temperature over N2 yields the oxide sulfate. Evaporation of neutral aqueous solutions provides basic sulfates. [J Am Chem Soc 55 1943 1933, 58 2126 1936.]... 

In a 1-L rbf attached to a Dean-Stark trap, equipped with a reflux condenser is placed distilled aniline (1, 46.5 g, 45.5 mL, 0.5 mol), commercially available ethyl acetoacetate (5, 65 g, 63.5 mL, 0.5 mol), benzene (100 mL) and glacial AcOH (1 mL). The flask is heated at about 125 °C, and the water which distills out of the mixture with the refluxing benzene is removed at intervals. Refluxing is continued until no more water separates (9 mL collects in about 3 hrs) and then for an additional 30 min. The benzene is then distilled under reduced pressure, and the residue is transferred to a 125 mL modified Claisen flask with an insulated column. The flask is heated in an oil or metal bath maintained at a temperature not higher than 120 °C while the forerun of 1 and 5 is removed and at 140-160 °C the product distills giving 78-82 g, 76-80% yield of 6. 

A solution of ( )-l,2-bis(trimethylsilyl)oct-l-ene (12mmol) in glacial AcOH (31 ml) and H20 (1.6 ml) was heated with stirring at 110°C for 29 h. The mixture was then cooled to0°C, aqueous NaOH (60 ml, 9 m) added, and the total was extracted with ether (50 ml). The ethereal extract was washed with saturated sodium hydrogen carbonate solution and brine, and dried. Concentration and distillation gave 2-trimethylsilyloct-l-ene (U.5mmol, 96%), b.p. 106 °C/1 mmHg. 

From a consistent set of hydrogenation enthalpies in glacial AcOH, the cyclooctadi-enes decrease in stability 1,5- (29) < 1, 4- (56) < 1,3- (55a) with sequential differences of 13.0 (29, 55a) and 6.7 (55a, 56) kJmol-1. For comparison—despite our earlier enunciated skepticism about isomerization reactions performed in polar media (Z-BuOK in DMSO) — the following enthalpies of reaction, and thus enthalpies of formation, differences were found43 16.4 1.4 and 2.8 0.8 kJmol-1. Consistency, if not precise numerical agreement, is found for the energetics of the isomeric cyclooctadienes. 

The synthesis of the title compound, 214, the active-site-directed photoaffinity radiolabel for androgen-binding proteins ( ABP ), has been accomplished180,181 by treatment of excess 17a-[( )-2-tributyltin(IV)ethenyl]androsta-4,6-dien-17 -ol-3-one, 215, with sodium iodide-125 of specific activity 27 Cimmol-1 in a sodium acetate-AcOH buffered solution and a solution of 30% H2O2 in glacial AcOH (equation 77). 

To 1 volume of the hydrazone mixture there was added, with mixing, 2 volumes of 0.6 M NaBH3CN in 0.1 M NaOAc/MeCN (1 1) the apparent pH was previously adjusted (glass electrode) to 4.6 with glacial AcOH. The apparent pH was readjusted to an apparent value of 4.6 with glacial AcOH, the soln incubated for 4d at rt in the dark, and the reduced hydrazone finally isolated by HPLC. The same conditions could be used for both the ligation steps shown in Scheme 2. 

A threefold excess of a 10 mM soln of H2NOCH2CO-Lys(FITC)-OH (10) in H20 containing 20% MeCN was added to the oxidized interleukin-8 soln (2 mg - mL 1 in 0.1 M NaOAc buffer, pH 4.6). MeCN was added to a final concentration of 10% to ensure solubilization of the reagent, and the pH of the soln was adjusted to 4.6 with glacial AcOH. After incubation for 15 h at rt in the dark, the product was purified from reactants by RP-HPLC on a C8 column. The coupling yield was estimated at 80% from the recovery of coupled protein. The conjugate had the expected molecular mass mlz calcd, 8941.6 found, 8940.6T1.0. 

Component A Glacial AcOH (5 mL) is added to HPLC grade water (1L). 

Tetrahydropyrano[3,2-r ]pyridazinone derivatives 741 were prepared from the reaction of atylhydrazonoacetyl-acetone 739 and PhCHO in glacial AcOH in the presence of NaOAc, in a single synthetic step, via the formation of diphenylheptadienearylhydrazone intermediate 740 (Equation 63) <1989IJB167>. 

Procedure for Determination of Nitrogen in Dinitroetbylbenzene. Transfer an accurately weighed portion of approx 0.5g of the sample to a 250-ml volumetric flask, make up to volume with glacial AcOH. and mix thoroughly. Avoid... 

Prepare on the day of test a soln of bromine-Na acetate—acetic acid soln by adding 10ml of bromine to 145ml of 10% soln of anhydrous Na acetate in glacial AcOH... 

Lumichrome [1086-80-2] M 242.2, m >290°. Recrystd twice from glacial AcOH and dried at 100° in a vacuum. 

N Acetyl-N-(2,4,6-trinitrophenyl)-hydrazine or Aeetylpicrylhydrazine, CHj.CO.HN.NH.-CfiH2(N02)3 It yel ndls (from ale), grn-yel prisms(from dil ale),- mp 210e](Ref 2), 223° (Refs 3 Sc 4) very diff sol in chlf eth, insol in pet eth. Can be prepd by heating pictyl hydrazine in glacial AcOH.No refs to its expl props... 

When the nitro compd was warmed with solvents, such as benz acet or glacial AcOH, brown fames of nitrogen dioxide were liberated. (See also Aminothiazoles)... 

Witt Witte prepd TNA by nitrating with coned nitric acid a soln of aniline in glacial AcOH (or in coned HaSO ) at about 5°, but the yields were poor. Better yields were obtained by... 

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