Synthesis, Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea

高等学校化学研究 ›› 2012, Vol. 28 ›› Issue (2): 230-233 .

Synthesis, Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea

ZHAO Dan¹, HUANG Jie¹, SONG Ji-rong², ZHONG Yi-tang¹, WANG Li-qin¹, HE Jian-yun¹

1. Shaanxi Key Laboratory of Physico-inorganic Chemistry, Department of Chemical Engineering,Northwest University, Xi'an 710069, P. R. China;
2. Conservation Technology Department, the Palace Museum, Beijing 100009, P. R. China

收稿日期:2011-08-03 修回日期:2011-10-26 出版日期:2012-03-25 发布日期:2012-03-08
通讯作者: HUANG Jie E-mail:huangjie@nwu.edu.cn
基金资助:
Supported by the National Natural Science Foundation of China(No.20571060) and the Natural Science Foundation of Shaanxi Province, China(No.2007B08).

Synthesis, Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea

ZHAO Dan¹, HUANG Jie¹, SONG Ji-rong², ZHONG Yi-tang¹, WANG Li-qin¹, HE Jian-yun¹

1. Shaanxi Key Laboratory of Physico-inorganic Chemistry, Department of Chemical Engineering,Northwest University, Xi'an 710069, P. R. China;
2. Conservation Technology Department, the Palace Museum, Beijing 100009, P. R. China

Received:2011-08-03 Revised:2011-10-26 Online:2012-03-25 Published:2012-03-08
Contact: HUANG Jie E-mail:huangjie@nwu.edu.cn
Supported by:
Supported by the National Natural Science Foundation of China(No.20571060) and the Natural Science Foundation of Shaanxi Province, China(No.2007B08).

摘要/Abstract

摘要： N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea was synthesized by the reacting of 2,3-dimethy- laniline, potassium thiocyanate(KSCN) and methyl chloroformate(ClCOOCH₃). Single crystal was obtained by slowly evaporation solvent at room temperature. The structure was characterized by elemental analysis, IR and X-ray crystalography. The compound crystallized: a triclinic system with space group Pī, a=0.83440(12) nm, b=0.89113(13) nm, c=0.93015(13) nm, α=76.548(2)°, β=63.906(2)°, γ=82.538(2)°, V=0.60379(15) nm³, Z=2, D_c=1.311 mg/m³, F(000)=252, μ=0.256 mm^-1, R₁=0.0379, wR₂=0.0919. The specific heat capacity of the title compound was determined by a Micro-DSC method, and the specific heat capacity was 1.25 J·g^-1·K^-1 at 298.15 K. Thermodynamic functions, relative to those at the standard temperature of 298.15 K, were calculated via thermodynamic relationship. The thermal behavior of the title compound under a non-isothermal condition was studied by differential scanning calorimetry/thermogravimetric(DSC/TG) method. There was an obvious endothermic peak in the DSC curve, the peak temperature was 479.43 K. The compound mass loss was 89.94% observed from the TG curve.

关键词: X-Ray diffraction, Acylthiourea, Crystal structure, Specific heat capacity, Thermal behavior

Abstract: N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea was synthesized by the reacting of 2,3-dimethy- laniline, potassium thiocyanate(KSCN) and methyl chloroformate(ClCOOCH₃). Single crystal was obtained by slowly evaporation solvent at room temperature. The structure was characterized by elemental analysis, IR and X-ray crystalography. The compound crystallized: a triclinic system with space group Pī, a=0.83440(12) nm, b=0.89113(13) nm, c=0.93015(13) nm, α=76.548(2)°, β=63.906(2)°, γ=82.538(2)°, V=0.60379(15) nm³, Z=2, D_c=1.311 mg/m³, F(000)=252, μ=0.256 mm^-1, R₁=0.0379, wR₂=0.0919. The specific heat capacity of the title compound was determined by a Micro-DSC method, and the specific heat capacity was 1.25 J·g^-1·K^-1 at 298.15 K. Thermodynamic functions, relative to those at the standard temperature of 298.15 K, were calculated via thermodynamic relationship. The thermal behavior of the title compound under a non-isothermal condition was studied by differential scanning calorimetry/thermogravimetric(DSC/TG) method. There was an obvious endothermic peak in the DSC curve, the peak temperature was 479.43 K. The compound mass loss was 89.94% observed from the TG curve.

Key words: X-Ray diffraction, Acylthiourea, Crystal structure, Specific heat capacity, Thermal behavior

ZHAO Dan, HUANG Jie, SONG Ji-rong, ZHONG Yi-tang, WANG Li-qin, HE Jian-yun. Synthesis, Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea[J]. 高等学校化学研究, 2012, 28(2): 230-233 .

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Synthesis, Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea

Synthesis, Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea

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