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1楼2016-07-27 22:06:09

keailinger

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你这个是手性产品吧，你要消旋体？

不坠青云之志

2楼2016-07-28 08:15:51

试炼LHQ

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2楼: Originally posted by keailinger at 2016-07-28 08:15:51
你这个是手性产品吧，你要消旋体？

我是手性的原料，做出来是手性产物

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3楼2016-07-28 08:17:50

keailinger

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试炼LHQ(流浪南昌代发): 金币+5, 感谢回帖 2016-08-08 14:49:30

3-氨基丁酸与氯化亚砜反应后，加乙醇成酯，然后硼氢化钾还原。得到3-氨基丁醇。

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不坠青云之志

4楼2016-07-28 08:17:57

woconan

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你原料是啥

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5楼2016-07-29 07:52:20

试炼LHQ

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4楼: Originally posted by keailinger at 2016-07-28 08:17:57
3-氨基丁酸与氯化亚砜反应后，加乙醇成酯，然后硼氢化钾还原。得到3-氨基丁醇。

我是用硼氢化钠还原的，但是提取时出问题，产物水溶性好，而且还原后处理有好多盐，除不掉

6楼2016-07-29 13:38:40

试炼LHQ

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5楼: Originally posted by woconan at 2016-07-29 07:52:20
你原料是啥

3-氨基丁酸

7楼2016-07-29 13:38:55

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

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