2-(2-ethoxyethoxy)ethanol

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:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 28.2 g. of 7-methyl-1-isopropyl-4-phenyl-5,6,7,8-tetrahydro-2(1H) quinazolinone, 9.6 g. of sulfur, 10 gms of sodium hydroxide, 20 gms of calcium chloride and 200 mls of carbitol (2-[2-ethoxyethoxy]ethanol) is heated under a nitrogen blanket at 150° C. for 2 hours. The resulting mixture is then cooled to 65° C., 500 mls. of benzene added and the mixture cooled with stirring to 15° C. and the liquid phase decanted. The organic phase is washed with water and evaporated to obtain an oil which is dissolved in a mixture of 100 mls of benzene and 100 mls of 50% aqueous hydrochloric acid. The resulting mixture is stirred for one hour at room temperature, the phases separated and the acid phase treated with 50 mls of benzene. The acid phase is neutralized with 50% sodium hydroxide solution, extracted with 150 mls of benzene and the benzene extracts washed with water until neutral. After drying over sodium sulfate, the benzene solution is evaporated to obtain the crude product which is recrystallized from ethylacetate to obtain 1-isopropyl-4-phenyl-7-methyl-2[1H]quinazolinone, m.p. 141°-142° C. A mixture of 28.2 g the mixture cooled the liquid phase decanted The organic phase is washed with water evaporated to obtain an oil which The resulting mixture is stirred for one hour at room temperature the phases separated the acid phase treated with 50 mls of benzene extracted with 150 mls of benzene the benzene extracts washed with water until neutral After drying over sodium sulfate the benzene solution is evaporated to obtain the crude product which is recrystallized from ethylacetate

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

実験手順: 2-(2-Ethoxyethoxy) ethanol, carbitol solvent, 129 g (0.96 m), 90 g (0.8 m) furoic acid and 1 g dibutyltin dioctoate were heated with xylene to remove water by azeotropic distillation to acid number 1.4. Zylene removed by distillation at a pot temperature of 200° and product distilled. Carbitol furoate was collected in fraction 2, 121°-125°, 91% carbitol furoate by gc. Yield of carbitol furoate 144 g, 79%. to remove water by azeotropic distillation to acid number 1.4 Zylene removed by distillation at a pot temperature of 200° and product distilled Carbitol furoate was collected in fraction 2, 121°-125°, 91% carbitol furoate by gc

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

実験手順: A 1,2,3,4-tetrahydrocarbazole-4-carboxamide or 4-carboxhydrazide (13) is dehydrogenated by refluxing in a solvent such as carbitol in the presence of Pd/C to produce the carbazole-4-carboxamide. Alternately, treatment of (13) with DDQ in an appropriate solvent such as dioxane yields carbozole (14).