1-碘庚烷

1-碘庚烷

1-Iodoheptane

4282-40-0

C7H15I

226.09800

0.00000

3.39180

226.02200

n20/D 1.490(lit.)

透明无色至淡黄色-橙色液体

174 °F

204 °C(lit.)

−48 °C(lit.)

1.379 g/mL at 25 °C(lit.)

immiscible

Stable at room temperature in closed containers under normal storage and handling conditions. May discolor on exposure to light.

Keep away from heat, sparks, and flame. Keep away from sources of ignition. Store in a tightly closed container. Store in a cool, dry, well-ventilated area away from incompatible substances. Store protected from light.

MJ1050000

3

29033080

S26-S36-S37/39

Xi

R36/37/38

2933990090

2933990090. 其他仅含氮杂原子的杂环化合物. 增值税率:17.0%. 退税率:13.0%. 监管条件:无. 最惠国关税:6.5%. 普通关税:20.0%

2933990090. heterocyclic compounds with nitrogen hetero-atom(s) only. VAT:17.0%. Tax rebate rate:13.0%. . MFN tariff:6.5%. General tariff:20.0%

<p>1.先将邻苯二酚与三氯化磷反应制成氯化亚磷酸邻亚苯酯,再与庚醇反应得到无色油状的亚磷酸酯。取上述亚磷酸酯50.9g(0.20mol)、50.8g(0.20mol)碘加入500ml二氯甲烷中,在室温搅拌1h。用10%硫代硫酸钠溶液洗液洗除可能存在的未反应的碘,再依次用5%NaOH溶液、5%NaHCO3溶液、饱和NaCl溶液洗涤,分出有机相,蒸除溶剂后,减压蒸馏,收集96-104℃(5.33-6.4kPa)馏分,得碘庚烷39g,收率86%。 <br>2.制法: 于装有搅拌器、回流冷凝器、滴液漏斗的反应瓶中,加入邻苯二酚110g(1.0mol),水浴冷却,剧烈搅拌下于15min内滴加三氯化磷206g(1.5mol),氯化氢气体不断逸出,反应体系逐渐固化。停止搅拌,室温放置1h。水浴加热至熔化,再搅拌反应2h。减压蒸馏,接受瓶用丙酮-干冰冷却,收集98℃/3.33kPa或91℃/2.399kPa的馏分,得氯化亚磷酸邻苯二酚酯165g,收率95%。冰箱中放置后固化,mp30℃。于2L反应瓶中加入上述氯化亚磷酸邻苯二酚酯<br>(2)87g(0.5mol),干燥的吡啶39.5g(0.5mol),无水乙醚500mL,冷至0℃,慢慢加入庚醇58.1g(0.5mol)与400mL无水乙醚的溶液,室温放置过夜。抽滤,滤饼用乙醚洗涤。合并滤液和洗涤液,蒸出乙醚,得无色油状亚磷酸酯127g。于装有搅拌器的反应瓶中,加入上述亚磷酸酯50.9g(0.2mol),干燥的二氯甲烷500mL,碘50.8g(0.2mol),室温搅拌反应1h。于分液漏斗中用10%的硫代硫酸钠洗涤至无碘的盐酸,再依次用5%的氢氧化钠、5%的碳酸钠、饱和氯化钠溶液洗涤。无水硫酸钠干燥。水浴蒸出溶剂,得粗品1-碘庚烷<br>(1)41.5g,收率92%。氮气保护下减压蒸馏。收集96～104℃/5.33～6.4kPa的馏分,得纯品<br>(1)39g,收率86%。 </p>

<p>用于有机合成。</p>