3,3'-dithiobis(propionohydrazide) synthesis
- Product Name:3,3'-dithiobis(propionohydrazide)
- CAS Number:50906-77-9
- Molecular formula:C6H14N4O2S2
- Molecular Weight:238.33
1609-40-1
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Yield:50906-77-9 70%
Reaction Conditions:
with hydrazine in ethanol at 85; for 5 h;
Steps:
The procedure of synthesizing DTPH was as follows. In brief, 3,3'-dithiodipropionic acid (10 g, 47.6 mmol), ethanol (22.1 g, 480 mmol) and p-toluenesulfonic acid (0.4 g, 2.1 mmol) were dissolved in toluene (30 ml). The reaction mixture was stirred for 24 h under reflux using a Dean-Stark trap, and the product dithiodipropionate diethyl was obtained after the reaction mixture was washed with NaHCO3 solution and water to pH 7. After this, dithiodipropionate diethyl (10 g, 37.5 mmol) and hydrazine (12 g, 240 mmol) were dissolved in ethanol (20 mL), and the mixture was stirred for 5 h at 85 °C to produce DTPH. Pure DTPH was obtained after the crude product was recrystallized from ethanol-water solution (5% v/v) three times. Yield: 70%, m.p. 131-132 °C. 1H NMR (DMSO-d6, δ ppm): 2.53 (t, -SCH2CH2-), 2.85 (t, -SCH2CH2-), 4.2 (s, -NH2), 9.1 (s, -NH-).
References:
Cui, Ning;Qian, Junmin;Xu, Weijun;Xu, Minghui;Zhao, Na;Liu, Ting;Wang, Hongjie [Carbohydrate Polymers,2016,vol. 136,p. 1017 - 1026]
15441-06-2
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50906-77-9
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1119-62-6
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50906-77-9
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