| 59% |
With triethylamine; In N-formyldiethylamine; at 20℃; for 168h; |
Example 1 Synthesis of 2,5-di-tertbutylimidazole 5.44g (0.04 moles) of 2,2-dimethylpropanimideamide hydrochloride were mixed with 7.2 g (0.04 moles) of 1-bromopinacolone and 11.2g of triethylamine in 16.0g of diethylformamide (DEF) and stirred at room temperature for 7 days. The reaction mixture was then poured into water and extracted three times with 50 ml units of hexane. The hexane fractions were combined and washed three times with 50 ml aliquots of water. The hexane layer was then stirred with 5g of anhydrous magnesium sulfate over night. The hexane was then removed by vacuum down to a volume of 5 ml to yield a fine suspension. This was filtered and the resulting solid washed with fresh hexane to yield 4.22g (59% theoretical) of colorless fine crystalline product, 99% pure by Gas Chromatography Mass Spectrometry gave a parent ion at 180 amu. Structure confirmed by X-ray crystallography (see Figure 1) GCMS. 1H NMR : (500 MHz, D8 THF): delta = 1.23 (s, 9H), delta = 1.3 (s, 9H), delta = 6.48 (s,1H), 5=10 (bs, 1H). 1H NMR : (500 MHz, D8 THF): delta = 30.3 (s, 3C), delta = 30.8 (s, 3C), delta = 32.1 (s, 1C), delta = 33.6 (s, 1 C), delta = 111 (bs, 1 C), delta = 148 (bs, 1 C), delta = 155 (s, 1 C). X-ray |
| 59% |
With triethylamine; In N-formyldiethylamine; at 20℃; for 168h; |
Example 1Synthesis of 2,5-di-tert-butylimidazole[001238] 5.44g (0.04 moles) of 2,2-dimethylpropanimideamide hydrochloride were mixed with 7.2 g (0.04 moles) of 1-bromopinacolone and 1 1.2g of triethylamine in 16.0g of diethylformamide (DEF) and stirred at room temperature for 7 days. The reaction mixture was then poured into water and extracted three times with 50 ml units of hexane. The hexane fractions were combined and washed three times with 50 ml aliquots of water. The hexane layer was then stirred with 5g of anhydrous magnesium sulfate over night. The hexane was then removed by vacuum down to a volume of 5 ml to yield a fine suspension. This was filtered and the resulting solid washed with fresh hexane to yield 4.22g ( 59% theoretical) of colorless fine crystalline product, 99% pure by GasChromatography Mass Spectrometry gave a parent ion at 180 amu. Structure confirmed by X-ray crystallography (see Figure 1 )H NMR : (500 MHz, D8 THF): delta = 1.23 (s, 9H), delta = 1.3 (s, 9H), delta = 6.48 (s,1 H), delta = 10 (bs, 1 H).H NMR : (500 MHz, D8 THF): delta = 30.3 (s, 3C), delta = 30.8 (s, 3C), delta = 32.1 (s, 1 C), delta = 33.6 (s, 1 C), delta = 11 1 (bs, 1 C), delta = 148 (bs, 1 C), delta = 155 (s, 1 C). |
| 59% |
With triethylamine; In N-formyldiethylamine; at 20℃; for 7h; |
Example 1; Synthesis of 2,5-di-tertbutylimidazole; 5.44 g (0.04 moles) of 2,2-dimethylpropanimideamide hydrochloride were mixed with 7.2 g (0.04 moles) of 1-bromopinacolone and 11.2 g of triethylamine in 16.0 g of diethylformamide (DEF) and stirred at room temperature for 7 days. The reaction mixture was then poured into water and extracted three times with 50 ml units of hexane. The hexane fractions were combined and washed three times with 50 ml aliquots of water. The hexane layer was then stirred with 5 g of anhydrous magnesium sulfate over night. The hexane was then removed by vacuum down to a volume of 5 ml to yield a fine suspension. This was filtered and the resulting solid washed with fresh hexane to yield 4.22 g (59% theoretical) of colorless fine crystalline product, 99% pure by Gas Chromatography Mass Spectrometry gave a parent ion at 180 amu. Structure confirmed by X-ray crystallography (see FIG. 1)GCMS.1H NMR: (500 MHz, D8THF): delta=1.23 (s, 9H), delta=1.3 (s, 9H), beta=6.48 (s, 1H), beta=10 (bs, 1H).1H NMR: (500 MHz, D8THF): delta=30.3 (s, 3C), beta=30.8 (s, 3C), beta=32.1 (s, 1C), beta=33.6 (s, 1C), beta=111 (bs, 1C), beta=148 (bs, 1C), beta=155 (s, 1C).X-ray |
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