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METHOD OF SYNTHESIS OF 2,6-DI-TERT-BUTYL-4-(3-HYDROXYPROPYL)-PHENOL

机译:2,6-二叔丁基-4-(3-羟丙基)-苯酚的合成方法

摘要

FIELD: organic chemistry. SUBSTANCE: 2,6-di-tert. -butyl-4-(3-hydroxypropyl)-phenol is synthesized by alkylation of 2,6-di-tert.-butylphenol with allyl alcohol at increased temperature and pressure, at mole ratio phenol:alcohol = 1:(1.2-2.0) for 3.5-4 h. The end product is separated from the vat residue by vacuum distillation. Catalyst: vat residue of distillation containing 3-(3.5-di-tert.-butyl-4-hydroxyphenyl)-propanol-1 sodium salt which is prepared preliminary by interaction of 2,6-di-tert.-butylphenol with sodium hydroxide at stirring and heating from 110 to 145 C with simultaneous distillation of water formed. Then mixture is cooled, mixed with allyl alcohol, and reaction is carried out for 3.5 h. Reaction mass is distilled under vacuum, and prepared vat residue is mixed with the parent reagents at the mass ratio phenol:vat residue = 3.85:1. After 3-4 reaction cycles all reactions beginning from catalyst preparing were repeated. Alkylated phenols were used in organic synthesis. EFFECT: improved method of synthesis.
机译:领域:有机化学。物质:2,6-二叔丁基。丁基-4-(3-羟丙基)-苯酚是通过在升高的温度和压力下,将烯丙基醇与2,6-二叔丁基苯酚烷基化而合成的,摩尔比为苯酚:醇= 1:(1.2-2.0)持续3.5-4小时。通过真空蒸馏将最终产物与桶残余物分离。催化剂:含有3-(3.5-二叔丁基-4-羟基苯基)-丙醇-1钠盐的蒸馏残余物,该盐是通过2,6-二叔丁基苯酚与氢氧化钠在250℃下相互作用而初步制备的搅拌并加热至110至145℃,同时蒸馏出水。然后将混合物冷却,与烯丙醇混合,并且反应进行3.5小时。在真空下蒸馏反应物料,并将制备的还原渣与母体试剂以苯酚:还原渣= 3.85:1的质量比混合。在3-4次反应循环后,重复从催化剂制备开始的所有反应。烷基化酚用于有机合成。效果:改进的合成方法。

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