Ethyl acetate ether

ACN, acetonitrile MeOH, methanol EtOH, ethanol BuOH, butanol EtOAc, ethyl acetate ether, diethyl ether HOAc, acetic acid DCM, dichloromethane DMF, dimethylformamide DMSO, dimethylsulfoxide. 

ACN, acetonitrile MeOH, methanol EtOH, ethanol PrOH, propanol BuOH, butanol EtOAc, ethyl acetate ether, diethyl ether pet. ether, petroleum ether HOAc, acetic acid DCM, dichloromethane THF, tetrahydrofuran TEA, triethylamine DMF, dimethylformamide TFA, trifluoroacetic acid TCA, trichloroacetic acid EDTA, ethylenediaminetetraacetic acid contg, containing soln, solution phosph., phosphate amm., ammonium. 

The solubility of nitroguanidine in organic solvents is limited. Desvergnes [31] determined its solubility in various solvents water, acetone, methyl and ethyl alcohols, ethyl acetate, ether, benzene, toluene, pyridine, chloroform, carbon tetrachloride and carbon sulphide. In all these liquids the solubility of nitroguanidine is negligible, the highest value—for pyridine—being 1.75 g/100 ml at 19°C. 

After further working up there is obtained an oily crystalline residue which is subjected to chromatography on silica gel. The 16a-methyl-6a,9a-difluoro-SM-pregnadien-lip l-diol-S O-dione is eluated with ethyl acetate-chloroform (1 2), it is recrystallized from ethyl acetate/ether and then formed to melt at 240°/242°-244°C. The yield is 60% of the theoretical. The product is reacted with valeric acid chloride to give the valerate ester. 

The 3-chloro-l-(4-indolyloxy)-2-propanol is dissolved in 50 ml of toluene and 50 ml of isopropylamine and heated to the boil for 45 h. Evaporation to dryness is effected in a vacuum, the residue is shaken out thrice between ethyl acetate and a 1 N tartaric acid solution and a 5 N sodium hydroxide solution is then added to the combined tartaric acid phases until an alkaline reaction is obtained. The alkaline solution is shaken out thrice with 50 ml of methylene chloride, the extracts are dried over magnesium sulfate and the solvent evaporated in vacuum. The residue is crystallized from ethyl acetate/ether to give the 4-(2-hydroxy-3-isopropylaminopropoxy)indole. 

Trimetaphosphimic acid, as the 2-hydrate, crystallizes as rectangular platelets which melt at 105 to 110° by a rapid determination. The solubility in water is approximately 111 g./lOO g. of water at 35°, and 48 g./lOO g. of water at 25°. The transition from 2-hydrate to anhydrous acid occurs at 33°. In the anhydrous form the acid crystallizes in characteristic rhombs which do not melt at 110° but decompose at higher temperatures. The crystals are not noticeably hygroscopic. Both forms are practically insoluble in alcohols, ethyl acetate, ether, or hexane. The x-ray diffraction patterns have been reported.1... 

The organic phase is dried over sodium sulfate, and solvent is removed by rotary evaporation to leave 1132 mg (97%) of the crude pale-yellow tripeptide. For further purification the crude product is dissolved in ethyl acetate, treated with some activated carbon and filtered through Celite. Removal of the solvent and crystallization from ethyl acetate/ether/petroleum ether (ca. 2 1 1) yields 993 mg (85%) of colorless crystals of benzyloxy-carbonyl-L-aspartyl-(tert-butyl ester)-L-phenylalanyl-L-valine methyl ester mp 119-120°C (Note 5). 

Hexamethyltri - 4 - aminotriphenylarsine oxide, [(CH3)aN. CgH jaAsO, is obtained from the hydroxide in white crystals, M.pt. 277 C. It dissolves readily in alcohols, is sparingly soluble in ethyl acetate, ether, or benzene, and is insoluble in water. 

Siloxycyclopropanes are also opened by platinum(II) complexes such as Zeise s dimer. - While 1-aryl-1-siloxycyclopropanes are transformed into P-platinum ketone complexes, 2-alkyl-substituted siloxycyclopropanes are isomerized cleanly to allyl silyl ethers in good yields. The reaction is quite general and proceeds with catalytic amounts of Zeise s dimer (2-10mol%) in many different suitable solvents (chloroform, dichloromethane, ethyl acetate, ethers, benzene) at ambient temperature with 100% inversion of configuration at the siloxy carbon and provides only silyl ethers of 2-methylene alkanols without contamination of doublebond isomers. ... 

First, with a favorable partition coeflScient, 2-5 volumes of extractant secure such a good recovery with one extraction that the use of repetitive slightly smaller volumes gains only a marginal increase in recovery at very considerable expense of time and effort. As Peterson (P6, P6a) first pointed out, one extraction of an aqueous solution of cortisol with 5 volumes of dichloromethane should, and in fact does, secure a recovery of 98% of the cortisol in the aqueous sample. Because of a preference for an upper layer extractant, my own work has usually employed one extraction with 5-6 volumes of ethyl acetate-ether, 1 2 by volume, for this class of steroids. In their double-isotope method for plasma testosterone and 17-ketosteroids, Gandy and Peterson (Gla) used one extraction with 9 volumes of dichloromethane-ethyl acetate, 1 1 by volume. Calculation will quickly show that with a partition coeflBcient of 10 in favor of the extractant, two extractions with three volumes will secure a recovery of 99.8% as compared with 98.4% using one extraction with 6 volumes. While it can be shown that with a random error of performance of the extractions the double extraction procedure will reduce the overall error in the recovery value, this is trivial compared with the extra labor in the extraction of many samples. If an internal radioactive... 

This compound, C iHaaNOg, crystallizes as bright yellow needles from ethyl acetate-ether, m.p. 235-237° (dec.), [a] -(-294° (chloroform) (296a). Polarographic and spectral evidence shows that Substance D does not contain a tropolone ring. It forms an oxime and an 0-acetyl derivative. Substance D is formed by the irradiation of Substance Ei and is converted to jS-lumicolchicine (lumicolchicine I, Substance I) by diazomethane (296a, 365). From these reactions and the evidence for the structure of jS-lumicolchicine, Substance D may be considered to have the partial formula CXXVIII. 

Dross of lead The oxidized scum which forms on the surface of melting lead. acetate 4291 C2HJC2H3O2 Acetate of oxide of ethyl acetic ether ... 

Needles from ethyl acetate, mp 138 (dec). The pure compound may be stored over P2Os for several months Crude material dec after a Tew hours Decomposed by hot water, acids or alkalies to COz and acelone K (25 ) 7.9 y 10- . Very sol in water and alcohol slightly sol in ethyl acetate, ether Insol in chloroform. Itgrom. benzene... 

Monohydrate, crystals from dilute acetone. Poor stability. Has no definite melting point. [ ] +9.5 (c — 4.7 in H,0), uv max (pH 7.0 phosphate buffer) 242, 274 nm (Ejjj, 321, 549). Freely sol in water. Somewhat sol in acetic acid, formamide, DMSO, aq solns of methanol, ethanol, acetone. Practically insol in anhydr alcohols, acetone, ethyl acetate, ether. LDM in rats 150 mg/kg (Thiersch). 

Orthorhombic crystals. Dec on heating, d 1.95. Freely sol in water sol in methanol slightly sol in ethanol, acetone almost insol in ethyl acetate, ether. 

Hydrochloride, C2SHmC1NjO, Scofaban. Crystals from ethanol + ethyl acetate + ether, mp 214-214.8°- LDM orally in mice 540 mg/kg (ealed as base). 

Pelmine, needles from water + acetone, dec 177". [u]f —11.5° (c = 2.81 in water). Sol in water, ethanol practically insol in acetone, ethyl acetate, ether. 

Dihydrate, prisms from water, mp 171 -173. [ ] +79.1" (water). Freely sol in water, methanol, ethanol, dioxane, acetic acid. Sparingly so] in ethyl acetate, ether and acetone. 

Form, prulaurasin. Slightly bitter needles from ethyl acetate + ether, mp 123-125". [a]D —54 (water). Soluble in water, alcohol practically insol in etheT. On hydrolysis yields d(-mandelic acid. 

Crystals from 50% ale, mp 74-75. So] in alcohol, ethyl acetate, ether. Practically insol in water, petr ether. 

Crystals from ether + hexane, mp 156-158. [ ] +93. uv max (ethanol) 227.5 nm (log e 4.10). Solvates easily and when crystallized from dilute acetone yields 1 cm long crystals of the acetone solvate. Soluble in alcohol, acetone, chloroform, benzene, ethyl acetate, ether. Slightly so] in water, dibutyl ether. Practically insol in hexane, aliphatic hydrocarbons. Compare also Picromycin. 

Hydrochloride. C HyCljNtOj. iVSC-245,382, ACNU, Nidran, White to light yellow cryst powder, uv max (0.041V HC1) 245 nm (E 480-510). Sol in methanol, slightly sol in abs ethanol, n-butanol. Practically insol in ethyl acetate, ether, chloroform, benzene, n-hexane. Gradually develops greenish yellow color in light decomposes slowly in humid air. LDM in mice, rats (mg/kg) 62, 46 i.v. (Masuda). 

Complex with creatinine sulfate, monohydrate, CMH2INS-O S.H.O, Antemovts. Plates. 215° dec. uv max (water at pH 3.5) 275 nm glacial acetic acid. Very sparingly sol in methanol, 95% ethanol. Insol in abs ethanol, acetoue, pyridine, chloroform, ethyl acetate, ether, benzene-... 

---