化学试剂
化學試劑
화학시제
CHEMICAL REAGENTS
2010年
1期
91-93
,共3页
杜葩%王红%高永红%金东元
杜葩%王紅%高永紅%金東元
두파%왕홍%고영홍%금동원
4,6-二甲氧基-2-氯嘧啶%氰乙酸叔丁酯%2-(4,6-二甲氧基)嘧啶乙腈%对甲苯磺酸%合成
4,6-二甲氧基-2-氯嘧啶%氰乙痠叔丁酯%2-(4,6-二甲氧基)嘧啶乙腈%對甲苯磺痠%閤成
4,6-이갑양기-2-록밀정%청을산숙정지%2-(4,6-이갑양기)밀정을정%대갑분광산%합성
2-chloro-4,6-dimethoxypyrimidine%tert-butyl cyanoacetate%2-(4,6-dimethoxypyrimidin-2-yl)acetonitrile%para-toluenesulfonic acid%synthesis
由4,6-二甲氧基-2-氯嘧啶与氰乙酸叔丁酯反应制备了2-氰基-2-(4,6-二甲氧基嘧啶基)乙酸叔丁酯,而后在对甲苯磺酸催化作用下,由2-氰基-2-(4,6-二甲氧基嘧啶基)乙酸叔丁酯脱羧制备了标题化合物.着重考察了不同反应时间、反应温度及物质的量比对目标产物产率的影响.较佳的合成条件为:n(对甲苯磺酸)∶n[2-氰基-2-(4,6-二甲氧基嘧啶基)乙酸叔丁酯]=0.08∶1,反应时间2 h,反应温度100 ℃,产物收率可达90%以上.化合物结构经IR、~1HNMR 、~(13)CNMR、MS进行了表征.
由4,6-二甲氧基-2-氯嘧啶與氰乙痠叔丁酯反應製備瞭2-氰基-2-(4,6-二甲氧基嘧啶基)乙痠叔丁酯,而後在對甲苯磺痠催化作用下,由2-氰基-2-(4,6-二甲氧基嘧啶基)乙痠叔丁酯脫羧製備瞭標題化閤物.著重攷察瞭不同反應時間、反應溫度及物質的量比對目標產物產率的影響.較佳的閤成條件為:n(對甲苯磺痠)∶n[2-氰基-2-(4,6-二甲氧基嘧啶基)乙痠叔丁酯]=0.08∶1,反應時間2 h,反應溫度100 ℃,產物收率可達90%以上.化閤物結構經IR、~1HNMR 、~(13)CNMR、MS進行瞭錶徵.
유4,6-이갑양기-2-록밀정여청을산숙정지반응제비료2-청기-2-(4,6-이갑양기밀정기)을산숙정지,이후재대갑분광산최화작용하,유2-청기-2-(4,6-이갑양기밀정기)을산숙정지탈최제비료표제화합물.착중고찰료불동반응시간、반응온도급물질적량비대목표산물산솔적영향.교가적합성조건위:n(대갑분광산)∶n[2-청기-2-(4,6-이갑양기밀정기)을산숙정지]=0.08∶1,반응시간2 h,반응온도100 ℃,산물수솔가체90%이상.화합물결구경IR、~1HNMR 、~(13)CNMR、MS진행료표정.
Tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl) acetate was prepared from 2-chloro-4,6-dimethoxypyrimidine and tert-butyl cyanoacetate.2-(4,6-dimethoxypyrimidin-2-yl) acetonitrile was further synthesized using tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl) acetate as raw material and para-toluenesulfonic acid as catalyst via decarboxylic reaction.Effects of reactant composition,reaction temperature and reaction time on the yield of 2-(4,6-dimethoxypyrimidin-2-yl)acetonitrile were investigated,and the optimal conditions were as follows:molar ratio of n[tert-butyl was 2 hours.The yield of 2-(4,6-dimethoxypyrimidin-2-yl)acetonitrile was above 90%.Meanwhile,structure of the product was characterized by IR,~1HNMR and ~(13)CNMR methods.
