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4-[4-(4-Nitro-2-sulfostyryl)-3-sulfophenylazo]-3-methyl-1-phenyl-5-pyrazolol condenses with p-phenylene diamine, p-aminobenzoic acid and sulfanilic acid respectively in dilute sodium hydroxide solution yielding disazo stilbene dyes which dye cotton directly in red-orange colors of different depth. Preliminary experiments show that the rate of condensation of sulfanilic acid with 4-[4-(4-Ni-tro-2-sulfostyryl)-3-sulfophenyl-azo]-3-methyl-1-phenyl-5-pyrazolol is slower than those of p-phenylene diamine and...

4-[4-(4-Nitro-2-sulfostyryl)-3-sulfophenylazo]-3-methyl-1-phenyl-5-pyrazolol condenses with p-phenylene diamine, p-aminobenzoic acid and sulfanilic acid respectively in dilute sodium hydroxide solution yielding disazo stilbene dyes which dye cotton directly in red-orange colors of different depth. Preliminary experiments show that the rate of condensation of sulfanilic acid with 4-[4-(4-Ni-tro-2-sulfostyryl)-3-sulfophenyl-azo]-3-methyl-1-phenyl-5-pyrazolol is slower than those of p-phenylene diamine and p-aminobenzoic acid. The properties of these condensation products and their methods of analysis are also described.

4-[4-(4-硝基-2-磺基苯乙烯)-3-磺基苯偶氮]-1-苯-3-甲-5-羟吡唑可和对苯二胺、对氨基苯磺酸及对氨基苯甲酸分别地在稀的氢氧化钠溶液中缩合成双偶氮二苯乙烯染料,后者能直接染棉織品成深度不同的杠橙色。对氨基苯磺酸和4-[4-(4-硝基-2磺基苯乙烯)-3-磺基苯偶氮]-1-苯-3-甲-5-羟吡唑在稀的氢氧化钠溶液中缩合的速度,较对苯二胺及对氨基苯甲酸为慢。本文还叙述了三种缩合产物的性质及分析方法。

1. The alkaloid contents of Chinese gelsemium (G. elegans Benth.) have been reinvestigated. Various procedures of isolation of the alkaloids were compared and a more efficient one developed. The present authors isolated besides previously reported koumine,kouminidine and gelsemine two new minor alkaloids:koumicine, m. p. 232-4°and koumidine, m. p.202-4°.However, sempervirine and kounidine were not obtained.Empirical formulae C_26H_30N_2O_4 and C_19H_22N_2O are provisionally assigned to koumicine and koumidine,...

1. The alkaloid contents of Chinese gelsemium (G. elegans Benth.) have been reinvestigated. Various procedures of isolation of the alkaloids were compared and a more efficient one developed. The present authors isolated besides previously reported koumine,kouminidine and gelsemine two new minor alkaloids:koumicine, m. p. 232-4°and koumidine, m. p.202-4°.However, sempervirine and kounidine were not obtained.Empirical formulae C_26H_30N_2O_4 and C_19H_22N_2O are provisionally assigned to koumicine and koumidine, respectively, and spectral evidences indicate that both these alkaloids are of indole type. The unconventional formula of kouminidine, C_19H_25O_4N_2, is revised to C_20H_26N_2O_4.Preliminary considerations based on UV and IR spectra suggest that kouminidine is possibly an indolenine type alkaloid with a zwitterionic structure.2. The constitution of koumine, the main alkaloid of Kou-Wen, has been preliminarily studied on spectral as well as on chemical ground. It is proposed that, in contrast to gelsemine, koumine probably possesses a pseudoindole ring system. Although gelsemine and koumine both contain an exo-vinyl, an Nb-methyl and most likely a cyclic ether linkage, the structures of the alicyclic parts of these two alkaloids appear also different from each other.

1.重研究了国产钩吻生物碱,比较和改良这些生物碱的提取方法.除获得前人曾经报告的钩吻素子、钩吻素卯和钩吻素甲以外,还得到了两种新的次要生物碱,钩吻素丁和钩吻素戊,但未得钩吻素丙和钩吻素辰.钩吻素丁熔点232-234°,实验式暂定为C_(26)H_(30)N_2O_4;钩吻素戊熔点202-204°,实验式暂定为C_(19)H_(22)N_2O;从紫外光谱推断,二者都是吲哚类型的生物碱.并修正钩吻素卯的实验式为C_(20)H_(26)N_2O_4,从紫外及红外光谱初步推测,它可能是一种内盐式的假吲哚类型生物碱. 2.对国产钩吻中的主要生物碱钩吻素子的化学结构作了初步解析.从光谱及化学证据推断,钩吻素子与钩吻素甲具不同的发色系统,前者属于假吲哚型,而后者已知是属于2-氧吲哚型的.虽然这两种生物碱都含环外乙烯基,N_b-甲基及可能具环醚结构,但是其脂环部分的构造按推断亦不相同.

The properties of cis-l,4-polybutadiene rubbers with different molecular weights which were obtained with titanium catalyst have been studied.The properties of raw cis-l,4-polybutadiene rubbers with different molecular weights are similar to each other with respect to (1) gel content, less than 1%, (2) cis-l,4-con-tent, 93-97%, and (3) glass temperature, -110 to -114℃ (Table 1A). However, the Mooney viscosity increases rapidly with [η] (Fig. 1). It is shown by stress-strain curves that all the cid-l,4-polybutadiene...

The properties of cis-l,4-polybutadiene rubbers with different molecular weights which were obtained with titanium catalyst have been studied.The properties of raw cis-l,4-polybutadiene rubbers with different molecular weights are similar to each other with respect to (1) gel content, less than 1%, (2) cis-l,4-con-tent, 93-97%, and (3) glass temperature, -110 to -114℃ (Table 1A). However, the Mooney viscosity increases rapidly with [η] (Fig. 1). It is shown by stress-strain curves that all the cid-l,4-polybutadiene samples under examination do not crystallize during stretching (Fig. 2).The behaviour of cis-l,4-polybutadiene in milling is very sensitive to temperature. Carbon black compoundings have been carried out on an open laboratory mill at cylinder temperatures of 25, 40, and 60 ℃, respectively. Smooth compounds from which vul-canizates with tensile strength over 200 kg/cm2 may be prepared can only be obtained at 25℃. When compounding is carried out at 40 or 60℃, cis-l,4-polybutadiene tends to crumble (Fig. 4), no smooth compound can be prepared, and the vulcanizate obtained loses tensile strength (Fig. 3).According to the following experimental results: (1) no gel formation, no significant degradation, and no change in microstructure can be observed when cis-l,4-poly-butadiene is masticated either at 25 ℃ or at 40 or 60 ℃ (Fig. 6 and Table 3); (2) the effect of temperature on milling is reversible (Table 4), it is presumed that the loss of tensile strength of the vulcanizate obtained from compound prepared at 40 or 60℃ is due to the difficulty of incorporation and dispersion of carbon black into the cis-1,4-polybutadiene rubber at a temperature above 40 ℃. This presumption is supported by the microscopic photographs of the cross-sections of the vulcanizates (Fig. 5).It is found that the tensile strength of the vulcanizate decreases rapidly as the modulus (M330%) exceeds 60 kg/cm2 (Fig. 8). However, with a suitable amount of sulphur to control the degree of cross-Hnking, vulcanizates of tensile strengths over 200 kg/cm2 can be obtained (Fig. 8 and Table 1B). The elastisity (Yerzley) and abrasive resistance of cis-l,4-polybutadiene vulcanizates are much better than those of natural rubber (Table IB).The effect of molecular weight of cis-l,4-polybutadiene on the mechanical properties of the vulcanizate has been investigated. It is found that vulcanizates of tensile strength around 200 kg/cm2 can be obtained within wide range of molecular weights ([η] 2.5 to 3.6), whereas elasticity increases with the [η] of the raw rubber (Fig. 9).

研究了用钛盐催化剂制备而具有不同分子量的顺-1,4-聚丁二烯的性貭。 各种具有不同分子量的顺-1,4-聚丁二烯生胶的性貭很相似:(1)凝胶含量低于1%,(2)玻璃化温度在—110至—114℃之间,(3)顺-1,4结构含量在93至97%(表1A)。但门尼粘度则随[η]值而激增(图1)。从生胶的应力-应变曲线可见各种顺-1,4-聚丁二烯样品在拉伸时并没有结晶现象(图2)。 顺-1,4-聚丁二烯在滚筒上的加工性能对配炼温度极敏感。在25℃,40℃和60℃滚筒温度下的加炭黑配炼试验中,发现唯有在25℃下配炼才得到光滑的混合物,由此可制得抗张强度超过200公斤/厘米~2的硫化物中,如果配炼系在40℃或60℃下进行,则顺-1,4-聚丁二烯趋向于破碎(图4),得不到光滑的混合物,由此而制得的硫化物丧失抗张强度(图3)。 根据下列试验结果:(1)将顺-1,4-聚丁二烯分别在25℃,40℃和60℃下进行素炼,在素炼过程中都不产生疑胶,无明显的降解(图6),又素炼后链节结构并无变化(表3);(2)温度对滚炼的影响是可逆的(表4)。我们认为,在40℃或60℃下配炼得到的硫化物之所以丧失抗张强度可能由于炭黑没有均匀分散。从合炭黑硫化...

研究了用钛盐催化剂制备而具有不同分子量的顺-1,4-聚丁二烯的性貭。 各种具有不同分子量的顺-1,4-聚丁二烯生胶的性貭很相似:(1)凝胶含量低于1%,(2)玻璃化温度在—110至—114℃之间,(3)顺-1,4结构含量在93至97%(表1A)。但门尼粘度则随[η]值而激增(图1)。从生胶的应力-应变曲线可见各种顺-1,4-聚丁二烯样品在拉伸时并没有结晶现象(图2)。 顺-1,4-聚丁二烯在滚筒上的加工性能对配炼温度极敏感。在25℃,40℃和60℃滚筒温度下的加炭黑配炼试验中,发现唯有在25℃下配炼才得到光滑的混合物,由此可制得抗张强度超过200公斤/厘米~2的硫化物中,如果配炼系在40℃或60℃下进行,则顺-1,4-聚丁二烯趋向于破碎(图4),得不到光滑的混合物,由此而制得的硫化物丧失抗张强度(图3)。 根据下列试验结果:(1)将顺-1,4-聚丁二烯分别在25℃,40℃和60℃下进行素炼,在素炼过程中都不产生疑胶,无明显的降解(图6),又素炼后链节结构并无变化(表3);(2)温度对滚炼的影响是可逆的(表4)。我们认为,在40℃或60℃下配炼得到的硫化物之所以丧失抗张强度可能由于炭黑没有均匀分散。从合炭黑硫化物断面的显微镜照片亦可看到在25℃下配炼的硫化物确不同于在40℃和60℃下配炼者(图5A)。 当含炭黑硫化物的定伸强度(M_(300%))超过60公斤/厘米~2

 
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