CN1039439C - 一种制备1,4-二硫代苏糖醇的方法 - Google Patents

一种制备1,4-二硫代苏糖醇的方法 Download PDF

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CN1039439C
CN1039439C CN93100416A CN93100416A CN1039439C CN 1039439 C CN1039439 C CN 1039439C CN 93100416 A CN93100416 A CN 93100416A CN 93100416 A CN93100416 A CN 93100416A CN 1039439 C CN1039439 C CN 1039439C
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dithio
dithiothreitol
weight
threose
alcohol
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CN1074718A (zh
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江幼岷
赵忠
潘和平
李鲁
陈士儒
戴昌世
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Institute of Radiation Medicine of CAMMS
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Abstract

本发明涉及一种化学物质的制备方法，目的是提供电解法来制备1.4-二硫代苏糖醇，该方法以4.5-二羟基-1.2-二硫环已烷为原料，在合成工艺中采用了电解还原法，阴极是汞、铜、铅金属，阳极是碳棒，稀盐酸为电解液，电解液温度在10-25℃之间。经电解还原而得到二硫代苏糖醇，该物质作为蛋白质的交联剂用在分子生物学方面。应用该法缩短了反应步骤，操作方便，避免了旧法中所需要的恶臭、有毒的硫代醋酸或硫化氢试剂。

Description

一种制备1,4－二硫代苏糖醇的方法
本发明涉及1.4-二硫代苏糖醇的一种制备方法。
1.4-二硫代苏糖醇(Dithiothreitol，简称DTT)，是DL-苏-1.4-二硫基-2.3-丁二醇异构体之一，通称Cleland试剂。国外报道了几种制备路线，但都离不开用具有恶臭，有毒的硫代醋酸或硫化氢，而且工艺操作也较复杂。(1.Evans RM.el at，：Dithiols Part III Dcrivatives ofpolyhydric alcohols.J Chem Soc 1949；248；2.Whitesidies GM.etal，：Rates of thiol-disulfide interchange reactions betweenmono-and dithiols and ellmans reagent.J Org Chem 1977；42(2)：332.3.Ciaudelli JP.Ger offen 2，.209，458 28 Sep 1972；US Appl 124，529 15 Mar 1971；(CA 1972；164016a)，国内未正式生产。
本发明的目的是找出一种操作方便、避免使用硫代醋酸或硫化氢试剂并且价格便宜的制备方法。
本发明提供了一条简便易行的新合成方法。以4.5-二羟基-1.2-二硫环己烷为原料电解而成。以汞、铜、铅等金属板为阴极，碳棒为阳极，5％(重量)的盐酸为电解液，电解完毕后用乙醚提取阴极液，回收乙醚得到1.4-二硫代苏糖醇。
Figure C9310041600031
本法制备1.4-二硫代苏糖醇有以下优点：
合成方法简便，容易掌握。用电解还原将4.5-二羟基-1.2-二硫环己烷还原成1.4-二硫代苏糖醇，容易进行，收率可以达到75％左右，副产物少，不需要真空蒸馏和重结晶处理就能达到纯度要求。
实施例：将4.5-二羟基-1.2-二硫环己烷9g(0.06M)置入烧杯中，加入150mm15％(重量)的盐酸为阴极液，以铅为阴极，5％(重量)的盐酸为阳极液，碳棒为阳极，素烧瓷简为隔膜，加入0.6g SnCl2到阴极液中，搅拌下通直流电，电流强度为3A，电压为5V，电解液温度控制在10-25℃，电解完毕后将阴极液脱色过滤，然后用乙醚分次提取，合并乙醚液并干燥，回收并蒸尽乙醚，即析出白色固体物，置入P2O5真空干燥器中，得白色疏松状固体7g，收率75.6％，熔点40-41℃，巯基的百分含量(SH％)为98.02。

Claims (2)

1.一种制备1.4-二硫代苏糖醇的合成方法，该方法以4.5-二羟基-1.2-二硫环己烷为原料，其特征是合成工艺中采用了电解还原法，阴极板是汞、铜、铅金属，阳极是碳棒、稀盐酸为电解液，电解液温度在10到25℃之间，电解完毕后用乙醚提取阴极液，回收乙醚后得到1.4-二硫代苏糖醇。
2.根据权利要求1所述的电解还原法，其特征为阴极液浓度为5％(重量)，阳极液浓度为5％(重量)。
CN93100416A 1993-02-04 1993-02-04 一种制备1,4-二硫代苏糖醇的方法 Expired - Fee Related CN1039439C (zh)

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CN103073462A (zh) * 2013-01-12 2013-05-01 江西师范大学 一种二硫苏糖醇的制备方法
CN115093352B (zh) * 2022-07-05 2024-04-26 湖南汇百益新材料有限公司 一种二硫苏糖醇的制备方法

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US4324625A (en) * 1979-08-14 1982-04-13 E. I. Du Pont De Nemours And Company Process for preparing alkanediols by electrochemical coupling of halohydrins

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4324625A (en) * 1979-08-14 1982-04-13 E. I. Du Pont De Nemours And Company Process for preparing alkanediols by electrochemical coupling of halohydrins

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