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zxc2022-01-12企业英语49

2. Experimental
2 。实验

All manipulations were carried out under nitrogen stan-
dard Schlenk techniques. Solvents were purified by stan-
dard procedures and distilled under nitrogen prior to use.
NMR spectra were recorded with a Bruker AMX 300 spec-
trometer. Infrared spectra were recorded with a Unicam
Mattson Model 7000 FTIR spectrophotometer using KBr
pellets. Elemental analyses were performed in our laborato-
ries (ITQB). Standard literature methods were utilized for
the preparation of [MoO2Cl2] [8], the 1,3-dialkyl-4,5-dim-
ethylimidazol-2-ylidenes were readily available by the
reduction of the corresponding imidazol-2(3H)-thiones
with potassium in boiling THF [9], while the 1,3-dibutyl-
4,5-dichloroimidazol-2-ylidene was obtained by deprotona-
tion of the corresponding imidazolium salts bytBuOK [10].
所有的操纵下进行了氮斯坦-
标准舒伦克技术。溶剂纯化斯坦-
标准程序,并根据氮蒸馏之前使用。
NMR谱录的布鲁克AMX 300规格
trometer 。红外光谱录与Unicam
马特森模型7000红外分光光度计使用溴化钾
微丸。元素分析进行了我们的实验室
里斯( ITQB ) 。标准文献的方法被用于
编写[ MoO2Cl2 ] [ 8 ] , 1,3 -二烷基- 4 ,5 -暗淡,
ethylimidazol - 2 - ylidenes有现成的
减少相应的咪唑-2 ( 3小时) ,硫酮
钾在沸腾四氢呋喃[ 9 ] ,而1,3 -二丁酯,
4,5 - dichloroimidazol - 2 -亚基得到deprotona -
化相应的咪唑盐bytBuOK [ 10 ] 。

2.1. Dichlorobis(1,3,4,5-tetramethylimidazol-2-ylidene)-
dioxomolybdenum(VI)MoO2Cl2(LMe)2(1)
2.1 。 双(三苯基磷)氯化镍 ( 1,3,4,5 - tetramethylimidazol - 2 -亚基) -
dioxomolybdenum (六) MoO2Cl2 (伦敦金属交易所) 2 ( 1 )

A solution of 1,3,4,5-tetramethylimidazol-2-ylidene
(0.74 g, 6.00 mmol) in THF (20 cm3) cooled to 20 °C,
was added to a suspension of MoO2Cl2(0.60 g, 3.00 mmol)
in THF (30 cm3) at 20 °C and the reaction mixture was
stirred for 1 h at low temperature. The product,
MoO2Cl2(LMe)2(1), immediately precipitated as a purple
powder directly from the reaction mixture, and was iso-
lated by filtration and washed twice with cold THF to yield
pure solid of 1 (1.14 g, 85%). Anal. Calc. for C14H24Cl2-
N4O2Mo (447.22): C, 37.60; H, 5.41; N, 12.53. Found: C,
37.52; H, 5.70; N, 12.10%. Selected IR data (KBr):
m(MoO) 942, 916 vs cm1.
一种解决办法的1,3,4,5 - tetramethylimidazol - 2 -亚基
( 0.74克, 6.00浓度)在THF (二十立方厘米)冷却至20 ℃ ,
添加到暂停MoO2Cl2 ( 0.60克, 3.00浓度)
在THF (三十○立方厘米)在20 ° C和反应混合物是
搅拌为1小时的低温。该产品,
MoO2Cl2 (伦敦金属交易所) 2 ( 1 ) ,立即沉淀为紫色
粉末直接从反应混合物,是异
lated过滤和清洗两次冷四氢呋喃,收益率
纯固体1 ( 1.14克, 85 % ) 。肛门。钙。为C14H24Cl2 -
N4O2Mo ( 447.22 ) : ć , 37.60 ;小时, 5.41 ;氮, 12.53 。发现: ć ,
37.52 ;小时, 5.70 ;氮, 12.10 % 。选定的红外数据(溴化钾) :
米(钼) 942 , 916与cm1 。