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barbarasong
铁杆木虫 (正式写手)
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wpsword8291: 金币+10, ★★★很有帮助 2013-03-19 15:31:11
wpsword8291: 金币+10, ★★★很有帮助 2013-03-19 15:31:11
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Example 3 （Beispiel 3） 2-phenyl-5,5-dimethyl-morpholine (Formula IIb) One part by weight of product from Example 2, is dissolved in 1.5mL/g (vaolume percent) conc.H2SO4. The mixture is stirred over night at room temperature, and then poured into ice. The solution is adjusted with NaOH to pH>7, and extracted with chloroform. The organic solution is distilled off, and then the residual oil is dissolved in HCl/alcohol solution. The HCl salt of 2-phenyl-5,5-dimethyl-morpholine is obtained. m.p is 165-168℃。m.p. of its picrate is 176-179℃。 |
3楼2013-03-19 15:06:28
barbarasong
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wpsword8291: 金币+20, 翻译EPI+1 2013-03-19 15:31:01
wpsword8291: 金币+20, 翻译EPI+1 2013-03-19 15:31:01
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Example 2 （Beispiel 2） 1-Phenyl-2-(a,a-dimethyl-ethanolamine)-ethanol (Formula !b) In a 3-necked flask with stirrer and addition funnel, 2mol 2-methyl-2-aminopropanol and 0.2mol H2O is charged. Under stirring, 1mol 2-phenyloxirane is dosed in. The reaction mixture is heated in a water bath until solidification. And then cooled by ice, ethanol os added and heated to reflux for several hours. During addition of light Petroleum ether, solid product is precipited. It can be crystallized in boiling water. m.p. is 142-143℃；m.p. of its picrate is 165-168℃。 |
2楼2013-03-19 15:00:05
