Procedure for synthesis of 1

Another two-step procedure for synthesis of 1 -Rp-isoquinohnes was reported by Pastor and Cambon. The cyclization step involves dehydration of amides 59 by... 

General Procedure for Synthesis of 1,2,3,4-Tetrahydro-P-carboline by Domino Copper-Catalyzed Three-Component Indole Formation and Cyclization with t-BuOK Synthesis of 2-Methyl-l-propyl-2,3,4,9-tetrahydro-lH-pyrido[3,4-hjindole (6a) and 2-Methyl-l-propyl-l,2,3,4-tetrahydropy-razino[l,2-a]indole (8a) (Table 1, Entry 11)... 

For aromatic or heteroaromatic monoaldehydes, ArCHO, an efficient procedure has been developed for synthesis of 1,3-dinitro compounds [132]. Rather than in situ reduction of O2, the O2 reduction is carried out in a divided cell with the aliphatic nitro compound as the solvent. Charge corresponding to 0.5 F with respect to the aldehyde is passed through the cell, the current is switched off... 

D. Lafont, P. Boullanger, O. Cadas, and G. Descotes, A mild procedure for preparation of 1,6-anhydro-jS-D-hexopyranoses and derivatives, Synthesis, (1989) 191-194. 

Reaction with trialkylboranes. Lane and Brown in 1971 reported a simple procedure for synthesis of highly substituted alcohols from trialkylboranes. For example, bromination of triethylboranc (1) under irradiation in the presence of water followed by oxidation with alkaline hydrogen peroxide gives 3-methyl-3-pentanol (2) in 88% yield. The reaction involves as the first step free-radical bromination in the a-position... 

Azoalkanes Timberlake ei al. recommend the following procedure for synthesis of azoalkanes (4) from N,N -dialkylsulfamides (1), Overall yields are 35-85%. 

Homoeyelic ring closures. Bunnett and Skorcz31 found that several aliphatic esters, nitriles, sulfones, and ketones bearing an m-o-chlorophenyl group react with potassium amide in liquid ammonia to form homocyclic products of ring closure by way of a benzyne intermediate. The procedure has since been modified to use sodium amide (commercially available).32 The reaction is probably the method of choice for synthesis of 1 -substituted benzcyclobutenes. 

Reaction with ketones (1, 369-370). Mock and Hartman3 have improved the original procedure for synthesis of /3-keto esters from ketones by using triethyl-oxonium fluoroborate as the Lewis acid catalyst rather than boron trifluoride. Thus cyclohexanone (1) is converted into 2-carboethoxycycloheptanone (2) in 90% yield under the new conditions the yield using BF3 was 38%. The reaction is... 

Intramolecular P-alkylation in a series of N-3-halopropyl amides of P(III) species presents a convenient alternative for the synthesis of different 1,2-azaphos-pholanes (Scheme 81) [176, 177], This procedure allowed synthesis of 1,2-azaphospholanes 122 and 130 containing amino acid residues as potential... 

Removal of water from certain compounds is often used for synthesis of aromatic rings. Adams and Hufferd977 obtained mesitylene from acetone by treatment with sulfuric acid, and Lyle et al.91s give the following generalized procedure for preparation of 1,3,5-triarylbenzenes ... 

A general procedure for synthesis of terminal episulfides of hexoses or hexitols consists in the action of potassium thiolacetate on an appropriately substituted 5,6-di-O-p-tolylsulfonyl derivative, followed by treatment of the resultant 6-(S-acetyl-6-thio-5-0-p-tolylsulfonyl derivative with cold, methanolic, sodium methoxide the reaction involves rearside attack on C-5 by the sulfur atom at C-6, to displace the p-tolylsulfonyloxy group with inversion.This procedure was used for the synthesis of 5,6-dideoxy-5,6-epithio-l,3 2,4-di-0-ethylidene-L-iditol (82), 5,6-dideoxy-5,6-epithio-l,2 3,4-di-0-isopropylidene-L-guUtol (83), and 5,6-dideoxy-5,6-epithio-1,2-0-isopropylidene-/3-L-idofuranose (84), from 1,3 2,4-di-0-ethylidene-... 

Intermolecular and intramolecular [3+2] cycloaddition reactions are among the most efficient and tvidely used procedures for synthesis of five-membered heterocycles. The reactive partners in these reactions are 1,3-dipoles and dipolarophiles such as alkenes and alkynes. 1,3-Dipoles vary in stability some can be isolated and stored, others are relatively stable, but they are usually employed immediately. Others are so unstable that they have to be generated and reacted in situ. There are tv ro general classes of dipole, often referred to as sp (Fig. 11.1) and sp -hybridized dipoles (Fig. 11.2). 

Intermediate 50 was subsequently heated under reflux in triisopropylbenzene (232 °C) for 1.5 to 20 h to provide the basic canthine skeleton 51. Recently, Lindsley et al. reported a rapid MW-mediated procedure for synthesis of 51 [95]. This reaction, performed in a monomode MW reactor at 180 °C, required a reaction time of only 5 min. Even more interesting, treatment of the acryl hydrazide-tethered indole input, with benzil in the presence of 10 equiv. NH4OAC delivered not only the expected triazine 50 but also, directly, the 1,2-diphenyl canthine derivative 51 (Scheme 17.37, reaction path b). The products were formed in a 9 1 ratio of 50 and 51, respectively. In the one-pot reaction, the indole underwent a three-component condensation to generate 50 followed by an intramolecular inverse-electron-demand Diels-Alder reaction and subsequent chelotropic expulsion of N2 to generate the 1,2-diphenyl canthine 51. 

An improvement employed the H202/MTO/fluorous alcohol system (described earlier) in a one-pot procedure for synthesis of mixed tetroxanes, which did not require isolation of the unstable and potentially explosive gem-dihydroperoxide intermediate 240. The more reactive carbonyl compound was first oxidized to the gi OT-dihydroper-oxide 240, followed by the addition of the less reactive carbonyl compound in the presence of 1 equiv of HBF4. This procedure afforded unsymmetrical tetroxanes 238 in good yields (method B, Scheme 45 Table 4) <2003TL6309>. 

Problem 11.13 Suggest ATRP procedures for synthesis of ABC-type triblok copolymers where A is polystyrene, B is poly(ferf-butyl acrylate), and C is poly(methyl acrylate) in one case (Case 1) and poly(methyl methacrylate) in another case (Case 2). 

General Procedure for Synthesis of S-Arylsulfonyl-2-ethy-nylaniline Synthesis of 2-Ethynyl-N-mesitylenesulfonylani-line (Ic)... 

General Procedure for Synthesi of 2-Ethynyl-N-methane-sufonylaniline Synthesis of 2-Ethynyl-N-methane sulfonyl-4-methoxycarbonylaniline (lb)... 

General Procedure for Synthesis of (Aminomethyl)isoquino-line-Fused Polycyclic Compounds by Domino Mannich-Type Reaction and Cascade Cyclization Synthesis o/6-/(N,N-Diisopropylamino)methyl]-3,4-dihydro-2H-pyrimido[2,l-SL] isoquinoline (12a) (Table 1, Entry 10)... 

In the study, we developed a convenient procedure for synthesis of CAPE analogues. As described in section 1, CAPE analogues have antimicrobial, anti-inflammatory, antioxidant, and antitumor activities (Kishimoto et al, 2005b). Finally, the CAPE analogues produced. 

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