[1]方永勤,武安邦.2,6-二异丙基-4-苯氧基苯基异硫氰酸酯的合成[J].常州大学学报(自然科学版),2012,(04):24-27.
　FANG Yong-qin,WU An-bang.Synthesis of 2,6-Diisopropyl-4-Phenoxyphenyl Isocyanate[J].Journal of Changzhou University(Natural Science Edition),2012,(04):24-27.
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2,6-二异丙基-4-苯氧基苯基异硫氰酸酯的合成()
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常州大学学报(自然科学版)[ISSN:2095-0411/CN:32-1822/N]

卷:
期数:
2012年04期
页码:
24-27
栏目:
出版日期:
2012-09-30

文章信息/Info

Title:
Synthesis of 2,6-Diisopropyl-4-Phenoxyphenyl Isocyanate
作者:
方永勤; 武安邦
常州大学 设计研究院,江苏 常州 213164
Author(s):
FANG Yong-qin; WU An-bang
Institute of Design and Research,Changzhou University,Changzhou 213164,China
关键词:
2; 6-二异丙基苯胺;  2; 6-二异丙基-4-苯氧基苯基异硫氰酸酯;  二(三氯甲基)碳酸酯;  Ullmann反应
Keywords:
2; 6-Diisopropylaniline;  2; 6-Diisopropyl-4-phenoxyphenyl isocyanate;  Triphosgene;  Ullmann condensation
分类号:
TQ 454.2
文献标志码:
A
摘要:
以2,6-二异丙基苯胺为原料,经溴化、Ullmann缩合、硫氰化得到2,6-二异丙基-4-苯氧基苯基异硫氰酸酯,并考察了反应条件对收率的影响。较优工艺为,溴化:-5 ℃,n(2,6-二异丙基苯胺):n(Br2)=1.00:1.05; Ullmann缩合:155 ℃,8-羟基喹啉铜为催化剂,n(2,6-二异丙基-4-溴苯胺):n(苯酚):n(KOH)=1.0:1.3:1.2; 硫氰化:70 ℃,n(BTC):n(硫代甲酸盐)=1.0:3.0,3步总收率82.2%。产品结构经IR、1H NMR谱确认。
Abstract:
2,6-Diisopropyl-4-phenoxyphenyl isocyanate was prepared by 2,6-diisopropylaniline via bromation, Ullmann condensation and thiocyanation reaction. The effects of reaction conditions were investigated, andthe optimal conditions were as follows, bromation: at -5 ℃,n(2,6-diisopropylaniline):n(Br2)=1.00:1.05; Ullmann condensation: at 155 ℃, copper 8-hydroxyquinoline as catalyst,n(2,6-diisopropyl-4-bromo aniline):n(phenol):n(KOH)=1.0:1.3:1.2; thiocyanation: at 70 ℃,n(BTC):n(dithiocarbamate)=1.0:3.0, total yieldafter three steps was 82.2%. All compounds obtained were identified by IR and1H NMR.

参考文献/References:

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备注/Memo

备注/Memo:
作者简介:方永勤(1966-),女,江苏姜堰人,研究员级高级工程师。
更新日期/Last Update: 2012-09-30