Heating, viii

Decomposition of VIII. Heating VIII neat at its melting point yielded IX mp 276°-278°C (Found C 56.9, H 5.1, N 17.3. Calc. (Ci5H16N404) C 57.0, H 5.1, N 17.7). Compound IX could also be synthesized from p-nitro-N-methylaniline and formaldehyde. 

Reagents i, Bu OK Bu OH MeOCH Cl ii, NBS PhCO ) iii, MeCOSK-CH,Cl, iv, HCI-MeOH v, trithian derivative of p-MeOCsH CHO-BFj-CH, Clj vi, CK-aq. MeOH-R.T. vii, Mel-NaH xylene-heat viii, —78 °C Bu jAlH-EtjO ix, (COClij-EtjO x, nO C-GHjClj xi, I mol BuLi 110°C xii, cone. HC1-70°C xiii, separate isomers xiv, -78 "C-Bu jAlH-THF xv, AcjO-pyridine xvi, iodosobenzene diacetate-MeCN MejS xvii, aq. NaOH-MeOH-R.T. xviii, w-ClCgH COjH xix, BFj-EtjO-CHjCL-R.T. 

V, Mg-EtBr vi, MeCHO vii, PhCH2Br-Mc2CO, heat viii, LiAlH4-THF ix, aq. HCl-MeOH x, MeC(OEt>3 pivalic acid, 140 °C xi, ClCOjEt-PhH, heat xii, aq. KOH, heat xiii, MeOH-HCl xiv, S-indolyl-CHjCOCl xv, saponify xvi, PPA, 80 °C xvii, MesCl-pyridine, 0 °C xviii, KCN-DMF, heat xix, CH2N2 XX, Oj-Pt-EtOAc... 

Reagents i, MeOH-EtjN, RT ii, aq. HCl-MejCO iii, CrOj-aq. H SO -Me CO iv, MeOH-HCl v, 3MeONa-MeOH-heat vi, hydrolysis (and -COj) vii, 2 o-aminobenzaldehyde-SNaOH-HaO, heat viii, mono-esterify ix, 240 °C, 0.3 CuO X, Etl-NaH, RT, DME xi, paraformaldehyde-dioxan-trace cone. H2SO4, 100 °C, xii, 1 aq. HjOj-Bu OK-Bu OH-DMSO... 

Fig. VIII-13. LEED and ESDIAD on clean and oxygen-dosed Ni(lll) (a) LEED, elean surface (b) H ESDIAD of NH3 on Ni(Ill), the halo suggesting free rotation of the surface NH3 groups (c) ESDIAD after predosing with oxygen, then heated to 600 K and cooled before dosing with NH3—only well-ordered chemisorbed NH3 is now present. (From Ref. 93.)...

Phenolsulphonephthalein (phenol red). Mix 10 g. of o-sulpho-benzoic anhydride (Section VIII,9), 14 g. of pure phenol and 10 g. of freshly fused zinc chloride in a small conical flask. Place a glass rod in the flask and heat gently over a flame to melt the phenol. Then heat the flask containing the well-stirred mixture in an oil bath at 135-140° for 4 hours. Stir from time to time, but more frequently during the first hour if the mixture froths unduly, remove the flask from the bath, cool and then resume the heating. When the reaction is complete, add 50 ml. of water, allow the water to boil and stir to disintegrate the product. Filter the crude dye with suction and wash it well with hot water. Dissolve the residue in the minimum volume of warm (60°) 20 per cent, sodium hydroxide solution, filter, and just acidify the filtrate with warm dilute hydrochloric acid (1 1). Filter the warm solution, wash with water, and dry upon filter paper. The yield of phenol red (a brilliant red powder) is 11 g. 

The flask was charged with 2.0 mol of dry, freshly distilled (note 1) methyl propargyl ether (VIII-6, Exp. 7), potassium iert.-butoxide (note 2) (5 g) was added with stirring and the mixture was heated under reflux. The reaction was... 

In the flask were placed 0.40 mol of dry, powdered copper(I) cyanide, 9 g of anhydrous lithium bromide (note 1), 50 ml of dry THF and 0.30 mol of l-bromo-2--heptyne (prepared from the corresponding alcohol and PBrs in diethyl ether, see VIII-2, Exp. 10). The mixture was heated until an exothermic reaction started, which occurred at about 80°C. The solid dissolved gradually. The mixture was kept... 

A polyether-amide with a heat distortion temperature of 198°C has been prepared by Hitachi by interfacial polycondensation of 2,2-bis-[4-(4-aminophen-oxy)phenyl]propane (VIII) with a mixture of isophthaloyl- and terephthaloyl-chloride (IX and X) (Figure 18.29). 

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