16019-33-3

基本信息
4,6-二氯-5-嘧啶乙醛
4,6-二氯嘧啶-5-乙醛
2-(4,6-二氯-5-嘧啶基)乙醛
2-(4,6-二氯嘧啶-5-基)乙醛
4,6-Dichloropyrimidine-5-acetaldehyde
4,6-Dichloro-5-pyrimidineacetaldehyde
5-PyriMidineacetaldehyde, 4,6-dichloro-
5-ACETALDEHYDEYL-4,6-DICHLOROPYRIMIDINE
5-Acetaldehydeyl-4,6-dichloropyrimidene
5-Acetaldehydehyl-4,6-dichloropyrimidine
(4,6-dichloro-5-pyriMidinyl)acetaldehyde
2-(4,6-Dichloro-5-pyrimidyl)acetaldehyde
4,6-Dichloro-pyriMidine-5-yl-acetaldehyde
物理化學(xué)性質(zhì)
制備方法

16019-31-1

16019-33-3
以5-烯丙基-4,6-二氯嘧啶為原料合成4,6-二氯嘧啶-5-乙醛的一般步驟如下:在配備磁力攪拌器的50 mL三頸燒瓶中,依次加入20 mL二氯甲烷和4,6-二氯-5-烯丙基嘧啶(5.0 g,0.026 mol),隨后加入二甲基亞砜(8 g,0.104 mol)和三乙胺。將反應(yīng)混合物冷卻至-40°C后,通入臭氧(O3)直至反應(yīng)溶液呈現(xiàn)藍(lán)色,此時(shí)停止臭氧通入并切換為氮?dú)猓∟2)保護(hù),持續(xù)30分鐘以徹底排除體系中的臭氧。接著,向反應(yīng)體系中加入硫脲(2.0 g,0.026 mol),并允許反應(yīng)混合物自然升溫至室溫。使用淀粉碘化鉀試紙檢測反應(yīng)體系,確認(rèn)無過氧化物存在(試紙不變藍(lán))。最后,向反應(yīng)混合物中加入60 mL水,并用二氯甲烷進(jìn)行兩次萃取。該步驟的收率為88%。
參考文獻(xiàn):
[1] Patent: CN108409745, 2018, A. Location in patent: Paragraph 0038; 0040; 0043; 0046; 0048; 0049; 0052
[2] Patent: WO2010/9195, 2010, A1. Location in patent: Page/Page column 76-77
[3] Patent: WO2010/9207, 2010, A1. Location in patent: Page/Page column 45
[4] Patent: WO2010/9208, 2010, A1. Location in patent: Page/Page column 73-74
[5] Patent: WO2011/62885, 2011, A1. Location in patent: Page/Page column 34