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试炼LHQ银虫 (小有名气)
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急求3-氨基丁醇工艺生产合成路线 已有2人参与
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bysjj888
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试炼LHQ(流浪南昌代发): 金币+5, 感谢回帖 2016-08-08 14:49:46
感谢参与，应助指数 +1
试炼LHQ(流浪南昌代发): 金币+5, 感谢回帖 2016-08-08 14:49:46
| General Procedure for the Synthesis of Compounds Starting from β-Amino Acids.; A solution of borane:tetrahydrofurane complex (1M, 3-4 mL per mmol=3-11 equiv. of β-amino acid) was added dropwise over a period of 1 hour to a cold (0° C.) suspension of beta amino acid (1 equiv.) in THF (1 mL per mmol). The mixture was stirred 20 minutes at room temperature at the end of the addition. It was then heated at reflux for 22 hours. The mixture was then cooled to 0° C.; and methanol (2 mL per mmol) was added over a period of 30 minutes. The mixture was then heated at reflux for 20 minutes and concentrated to a thick oil. The oil was co-evaporated with methanol (3.x.200 mL). The solid obtained was dried in vacuo to afford the coresponding 3-substituted 3-amino-1-propanol derivative as a white waxy solid (quantitative yield). An aqueous solution of HBr (48percent, 2 mL per equiv. of the alcohol) was added slowly to a flask containing a 3-substituted 3-amino-1-propanol (1 equilv.). The mixture was heated at reflux for 6 hours, and then concentrated to dryness. The crude material was used directly in the next step. The 1-substituted 3-bromo-1-propylamine hydrobromide (obtained in step 2) was added to a solution of sodium sulfite (1.0 equiv. of the 1-substituted 3-bromo-1-propylamine) in water and 1,4-dioxane. The mixture was heated under reflux for 6 h then concentrated to dryness. The residual material was treated with concentrated HCl. The inorganic material was removed by filtration; and the filtrate was treated ethanol, causing precipitation of the corresponding sulfonic acid. The crude sulfonic acid was suspended in ethanol and the mixture was heated at reflux for 1 hour. After cooling to room temperature, the solid material was collected by filtration, rinsed with ethanol and dried overnight in the vacuum oven at 60° C., giving the corresponding 3-substituted 3-amino-1-propanesulfonic acid as a fine white crystalline solid. 这个或许对你有用 |
8楼2016-07-29 16:58:55
keailinger
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2楼2016-07-28 08:15:51
试炼LHQ
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3楼2016-07-28 08:17:50
keailinger
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4楼2016-07-28 08:17:57
