1,1,2-trichloroethene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2.57 g of ethyl 1-cyclopropyl-5,6,7-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate, 1.8 ml of benzylamine and 180 ml of trichloroethylene was heated under reflux for 3 hours and 40 minutes. Water and 10% hydrochloric acid were added to the reaction mixture to render the aqueous layer acidic. The trichloroethylene layer was separated and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was separated and purified by silica gel column chromatography to give 2.78 g of ethyl 5-benzylamino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxlate. m.p. 144°-145° C. was heated under reflux for 3 hours and 40 minutes The trichloroethylene layer was separated dried over anhydrous sodium sulfate The solvent was evaporated under reduced pressure the residue was separated purified by silica gel column chromatography

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The solutions useful in the method of the present invention include those obtained by a combination of a polyolefin and a petroleum hydrocarbon such as benzene, toluene, xylene, solvent naphtha or the like or a chlorinated hydrocarbon such as trichloroethylene, tetrachloroethylene, dichloroethane, dichloroethylene or the like. Low density polyethylene, medium density polyethylene, high density polyethylene, atactic (amorphous) polypropylene, isotactic (crystalline) polypropylene, ethylene-propylene copolymer, propylene-butylene copolymer can be mentioned as useful polyolefins. It is preferable to use a solution having a gelation point of 40°-60° C at a concentration in the range of 1-5% by weight. However, among the above-mentioned, a combination of benzene (b.p. 80.1° C), cyclohexane (b.p. 80.7° C), dichloroethylene (b.p. 83.5° C) with a resin other than atactic polypropylene is not of practical value because of poor solubility. Though tetraline (b.p. 210.5° C) or kerosene (b.p. 150°-320° C) provides nice gel-forming property, they are the examples which are not useful on account of too high boiling point. For the foregoing reason, toluene, xylene and tetrachloroethylene are preferable as a solvent for polyolefins and inflammable tetrachloroethylene is most suitable if safety is also taken into consideration. a gelation point of 40°-60° C at a concentration in the range of 1-5% by weight

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 41.3 g of a crude 5-nitronaphthoquinone cake (having a water content of 40 wt% and a dry weight of 24.8 g, and comprised of 75 wt% of 5-nitronaphthoquinone and 15 wt% of 6-nitronaphthoquinone when determined under dried conditions), 13.1 g of 1,3-butadiene and 124 g of trichloroethylene were introduced into an autoclave. The autoclave was hermetically sealed and the reaction was effected at 80°C for 2.5 hours. Then, Example 1 was repeated to obtain 20.7 g of 5-nitrotetrahydroanthraquinone. The yield was 88.0%. The thus obtained 5-nitrotetrahydroanthraquinone was oxidized and reduced in accordance with the standard method to obtain 1-aminoanthraquinone having a purity above 98 wt% and a 2-aminoanthraquinone content of 0.5 wt%. were introduced into an autoclave The autoclave was hermetically sealed

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture containing 131.5 g (1.0 mole), of trichloroethylene, 80.5 (0.5 mole) of 3,4-dichlorotoluene and 5 g. of aluminum chloride was stirred and heated at reflux for 2 hours. The reaction mixture was then washed with concentrated HCl, then with water until neutral, dried and distilled. 42.7 grams of product was collected, having a boiling point of 97°-102°C at 0.5 mm Hg pressure. A mixture containing 131.5 g (1.0 mole) heated at reflux for 2 hours The reaction mixture was then washed with concentrated HCl with water until neutral, dried distilled 42.7 grams of product was collected