X-ray, diffraction studies on protein fibers I The large fiber-axis period of collagen
X-ray, diffraction studies on protein fibers I The large fiber-axis period of collagen
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DOI：
10.1021/ja01236a027
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发表时间：
1944-07-01
影响因子：
15
通讯作者：
Bear, RS
中科院分区：
文献类型：
--
作者：
Bear, RS
3.4-二氯苯乙烯--将150克3，4-二氯苯甲基甲醇、1.5克对苯二酚和1.5克硫酸氢钾的混合物置于500毫升的容器中。改进的克莱森烧瓶，浸入210-215℃的油浴中。压力从最初的110毫米逐渐降低到15-20毫米。其中，苯乙烯-水混合物在130-150℃蒸馏。按常规方法处理产品后，得到90克(83%)的3，4-二氯苯乙烯，沸腾温度为69-70(4 Mm)，dm4为1.256，m20d为1.5857。警方回收了31克甲醇。肛门。卡尔德。对于C8H6C12：C，55.48；H，3.47。发现：C，55.72；H，3.71.2，5-Dichlorophenylmethylcarbinol.—2-Chloro-5-nitro-benzaldehyde按Erdmann方法制备。2，5-二氯苯甲醛从110g中得到110g(83%)的2，5-二氯苯甲基甲醇，第107-109页(2 Mm)；第63页。
3.4-Dichlorostyrene.—A mixture of 150 g. of 3, 4-dichlorophenylmethylcarbinol, 1.5 g. of hydroquinone, and 1.5 g. of potassium bisulfate was placed in a 500-cc. modified Claisen flask and immersed in an oil-bath held at 210-215. The pressure, initially at 110 mm., was gradually reduced to 15-20 mm. where thestyrene-water mixture distilled at 130-150. After working up the product in the usual manner there was obtained 90 g.(83%) of 3, 4-dichlorostyrene boiling at 69-70 (4 mm.); dm4 1.256; m20d 1.5857. Thirty-one grams ofcarbinol was recovered. Anal. Calcd. for C8H6C12: C, 55.48; H, 3.47. Found: C, 55.72; H, 3.71.2, 5-Dichlorophenylmethylcarbinol.—2-Chloro-5-nitro-benzaldehyde was prepared according to the method of Erdmann. 19 Thenitro group was reduced and replaced by chlorine'exactly as described for the preparation of m-chlorobenzaldehyde in “Organic Syntheses.” 11 From 110 g. of 2, 5-dichlorobenzaldehyde there was obtained 110 g.(83%) of 2, 5-dichlorophenylmethylcarbinol, b. p. 107-109 (2 mm.); m. p. 63-64.