Orange powders

Antimony Trisulfide. Antimony(III) sulfide (antimony sesquisulftde) [1345-04-6] SbS, exists as a black crystalline soHd, stibnite [1317-86-8] and as an amorphous red to yeUow-orange powder. Stibnite melts at 550°C and has Ai i° 298 175 kJ/mol (—41.8 kcal/mol)) A°29g, 182 J/(182 mol-K) [43.5 cal/(43.5 mol-K)] for the amorphous soHd AH° 298 1 147 kJ/mol (—35.1 kcal/mol) (38). The crystal stmcture of stibnite contains two distiucdy different antimony sites and consists of two parallel Sb S chains that are linked together to form cmmpled sheets (two per unit cell). 

To a gently swirled solution of the crude amine in 54 ml. of methanol is added 54 ml. (123 g., 0.87 mole) of methyl iodide. The solution is heated on a steam bath for 5 minutes and cooled to room temperature, and 800 ml. of ether is added. The meth-iodide, which separates as an oil, crystallizes on being scratched. The solid is collected on a Buchner funnel, washed with ether, and dried at 20-50 mm. for several hours at room temperature to yield 65-78 g. (68-81% Note 8) of N,N-dimethylaminomethyl-ferrocene methiodide as an orange powder, m.p. 200° (dec.) (Note 9). 

Observable Characteristics - Physical State (as normally shipped) Solid Color Yellow-orange (powder), dark gray (flakes), yellow brown Odor None. 

Thermolysis of the hexamethyl-substituted Dewar benzene-phenylazide adduct 1 in refluxing Decalin affords the 1.2,3-triazonine derivative 2 as the major product in form of a yellow-orange powder.30 A bicyelic isomer is also isolated which arises from rearrangement of 2 by purification on alumina and is readily converted back to 2 on heating to 80 C. 

Orange Powders. Various BlkPdrs manufd in the last century by Laflin and Rand Powder Co at Orange, NJ, USA. Also see under Laflin and Rand Powder Co in Vol 7, L2-R Ref Daniel (1902), 400... 

Under nitrogen, anhydrous DMF (10 mL) was added to a mixture of 83 (0.240 g, 0.5 mmol), 84 (0.063 g, 0.5 mmol), and Et3N (1 mL). Pd(PPh3)4 (0.027 g, 0.025 mmol) and Cul (0.005 g, 0.025 mmol) were then added and the reaction mixture was stirred at 100°C for 48 h. After being cooled to room temperature, die reaction mixture was poured into MeOH and filtered. The solid was washed with MeOH and dried under vacuum. The repetition of the precipitation procedure gave polymer 85 as orange powder in 96% yield (0.212 g). GPC (polystyrene standards) Mn — 15.100. 

The above-mentioned method is useful but metals that form strong M-S bonds (e.g., Hg, Ag, Sn) do not dissolve in W-Melm solutions of sulfur. This problem has been solved by the addition of Mg to the reaction mixture. Metal polysulfides having a variety of metals can be synthesized by the 7 T-Melm/ M-i-Mg/Sg method (Scheme 11) [48]. For example, a mixture of Mg, Sb powder (1 eq.), Sg (15 eq. as S) and W-Melm is heated at 80 °C for 48 h to afford the orange powder of [Mg(N-MeIm)5]Sb2Sj ( x 15) in 88% yield. Rauchfuss et al. proposed the mechanism of these reactions as follows. First, the reduction of Sg with Mg occurs to give the [Mg(W-MeIm)6] salt of Sg , which is probably in equilibrium with Sg, Ss ", Ss" and other species. Independently, the sulfuration of the thiophilic metal takes place. Next, the polysulfide an-... 

Other properties Munsell color yellow-orange powdered solid density 1.41 g mL log Kan 4.1, thermally stable... 

Human life, furthermore, certainly benefits from a less polluted world, and here, again, sol-gel entrapped catalysts are, literally, able to have transferred to within their large inner porosity the whole chemistry of fine chemicals production. Think for instance of an innocuous easily handled orange powder called SiliaCat TEMPO (Chapter 5) that added to a mixture of alcohols at 0 °C with a modest excess of aqueous, cold bleach rapidly converts them into all those fragrances, vitamins, hormones and drugs made of carbonyl compounds. 

The Ir(III)-amido-hydrido complex 43 was isolated by reacting the electron-rich neutral phosphine-cyclooctene complex 42 according to Equation 6.13 [7] (note the cis arrangement of the hydride and amide function). Likewise, the cationic complex 44 reacted in neat aniline to afford a 50/50 mixture of the N—H (45) and C—H (46) activation products that was isolated as a light orange powder (Equation 6.14). Compound 45 was separated from 46 and purified in 49% overall yield. 

Arsenic disulfide (AsS) is also known as ruby arsenic because it is a reddish-orange powder. It is used as a depilatory agent, a paint pigment, and a rat poison and to make red glass and fireworks. 

Ethyl (6-Methoxy-l,2-naphthoquinonyl-6) Cyanoacetate. The above naphthoquinone (21.7 g) is added to a solution of 500 cc of ethanol and 14 cc of ethyl cyanoacetate, followed by the addition of 32 cc triethylamine. A deep purple color will develop and the mixture should be swirled for 4 min to dissolve the quinone completely. A solution of 75.9 g of potassium ferricyanide in 320 cc of water is then added to the solution, causing a thick dark complex to form and separate. Redissolve by adding a soluhon of 24 g of sodium carbonate in 1,600 cc of water. Swirl or stir and filter through diatomaceous filter aid. Acidify the filtrate with 100 cc of 6 M sulfuric acid to precipitate 34.8 g of red-orange powder, which is oven dried at 70°. Reciystallize from ethyl acetate to get 19.3 g, mp 157-158.5°. The remaining filtrate is evaporated to a small bulk and reciystallization from ethyl acetate gives an additional 2.8 g of product. 

Physical Form. Yellow to brown or orange powder or flakes... 

B. 7-Fluoroisatin (3). A 250-mL, three-necked, round-bottomed flask fitted with a condenser and a thermometer is charged with 100 mL of coned sulfuric acid. After heating to 70°C, 30.0 g (0.165 mol) of anilide 2 (Note 9) is added over a period of 1 hr. The resulting deep red solution is heated to 90°C (Note 10) for 60 min (Note 11) and then is cooled to room temperature (20°C) over an ice bath (Note 12). The mixture is then added rapidly to a vigorously stirred mixture of 1.0 L of ice water and 200 mL of ethyl acetate (Note 13). The organic phase is separated and the almost black aqueous phase is extracted twice with 200 mL of ethyl acetate (Note 14). The combined red organic phases are dried with sodium sulfate. The solvent is removed under reduced pressure and the crude product is dried at low pressure, whereupon 12.9 to 15.7 g (47-57%) of an orange powder, mp 186-190°C, is obtained (Note 15). The crude product is sufficiently pure for the next step. Further purification is possible by recrystallization from acetone/water. 

White crystalline powder orthogonal crystal system the tetrahydrate is a yellow-to-orange powder which, on heating at 180°C, loses aU molecules of water density of tetrahydrate 3.91 g/cm anhydrous salt decomposes at 350°C forming Ce0S04 soluble in water (decomposes) soluble in dilute H2SO4 and other concentrated mineral acids. 

Realgar (arsenic disulfide, AsjSj) is an orange powder with a melting point of 308°C and a boiling point of 565°C [2]. Due to its low boiling point, it has been used in yellow smoke compositions (in spite of its toxicity ), and has also been used to aid in the ignition of difficult mixtures. 

The red crystalline (orange powder) MnI(CO)s is more soluble in common organic solvents thatn the chloro analogue. It dimerizes slowly in solution. The... 

As early as 1963 Markl prepared the first representatives of this class of compounds via multi-step synthesis l,l-diphenyl-X -phosphorin 118 ( 1,1-diphenyl-phosphabenzene ) and 1,l-diphenyl-2,3-benzo-X -phosphorin i20 ( 1,1-diphenyl-phospha-naphthalene ). Neither compound could be obtained in crystalline form. Instead, treatment of the crystalline phosphonium salts iiP and 121 with aqueous alkali affords very reactive, air-sensitive yellow or orange powders 118 and 120). Acid treatment leads back to the phosphonium salts. 

The layers were separated and the aqueous phase was extracted with dichloromethane (2 X 10 mL). The combined organic extracts were dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The red/brown residue was purified by column chromatography (eluent dichloromethane) to give the desired iridium complex (262 mg, 0.15 mmol, 68%) as an orange powder. 

Methylquinoline (2.86 g, 20 mmol) is added to a stirred suspension of palladium acetate (4.48 g, 20 mmol) in dichloromethane (150 mL) in a 250-mL beaker. The mixture is stirred for 4 h at room temperature. The brown solution is then filtered and the solution is dried in vacuo. The oily residue thus obtained is washed with diethyl ether (10 mL) and then with pentane (4 x 50 mL) to give 5.9 g (96%) of the acetato-bridged dimer as an orange powder. It can be crystallized from a chloroform-diethyl ether solution as deep yellow crystals. 

Table I. Emulsion Size of Spray Dried Orange Powders...

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