2,3-二甲基环己醇

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In 5 ml of tetrahydrofuran was suspended 0.19 g of sodium hydride (60% in oil), to which 0.5 ml of a tetrahydrofuran solution containing 0.48 g of 2,3-dimethylcyclohexanol (mixture of isomers) was slowly added dropwise with stirring at room temperature. The mixture was stirred at room temperature for 10 minutes and then cooled to 0° C., to which 1.5 ml of a tetrahydrofuran solution containing 0.5 g of 4,6-dichloropyrimidine was slowly added dropwise, followed by further stirring at room temperature for 3 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution and extracted three times with t-butyl methyl ether. The organic layers were combined, washed with brine, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.72 g of 4-chloro-6-(2,3-dimethylcyclohexyloxy)pyrimidine. was slowly added dropwise The mixture was stirred at room temperature for 10 minutes was slowly added dropwise by further stirring at room temperature for 3 hours extracted three times with t-butyl methyl ether washed with brine dried over anhydrous magnesium sulfate concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In 5 ml of tetrahydrofuran was suspended 0.19 g of sodium hydride (60% in oil), to which 0.5 ml of a tetrahydrofuran solution containing 0.48 g of 2,3-dimethylcyclohexanol (mixture of isomers) was slowly added dropwise with stirring at room temperature. The mixture was stirred at room temperature for 10 minutes and then cooled to 0° C., to which 1.5 ml of a tetrahydrofuran solution containing 0.5 g of 4,6-dichloropyrimidine was slowly added dropwise, followed by further stirring at room temperature for 3 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution and extracted three times with t-butyl methyl ether. The organic layers were combined, washed with brine, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.72 g of 4-chloro-6-(2,3-dimethylcyclohexyloxy)pyrimidine. was slowly added dropwise The mixture was stirred at room temperature for 10 minutes was slowly added dropwise by further stirring at room temperature for 3 hours extracted three times with t-butyl methyl ether washed with brine dried over anhydrous magnesium sulfate concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 50.7 g (0.5 mol) sec.-Butyl isocyanate were placed in a 500 ml vessel at ambient temperature and 64.1 g (0.5 mol) 2,3-dimethylcyclohexanol were added. The reaction mixture was heated for 5 h to 150° C., cooled and subsequently 100 ml water were added. After refluxing for one hour the solution was cooled down, the phases separated and extracted once with MTBE (methyl tert.-butyl ether). The raw product was purified by distillation to yield 60.2 g product as a mixture of isomers with a purity of 99.6%. The reaction mixture was heated for 5 h to 150° C. cooled After refluxing for one hour the solution was cooled down the phases separated extracted once with MTBE (methyl tert.-butyl ether) The raw product was purified by distillation