摘要
首先,选用硝基烷与醛反应,合成了4-硝基-3-己醇,3-硝基-4-庚醇及2-硝基-1-苯基丙醇,经铁粉还原得到4-氨基-3-己醇、3-氨基-4-庚醇及2-氨基-1-苯基丙醇。然后,以三乙胺为缚酸剂,以氨基醇、酮(或醛)和二氯乙酰氯为原料,合成了6个二氯乙酰基口恶唑烷类潜在的除草剂安全剂,分别为N-二氯乙酰基-2,2,4-三甲基-1,3-口恶唑烷、N-二氯乙酰基-4-甲基-2-丙基-1,3-口恶唑烷、N-二氯乙酰基-3-甲基-1-氧杂-4-氮杂螺[4.5]癸烷、N-二氯乙酰基-2,3-二乙基-1-氧杂-4-氮杂螺[4.5]癸烷、N-二氯乙酰基-3-乙基-2-丙基-1-氧杂-4-氮杂螺[4.5]癸烷及N-二氯乙酰基-3-甲基-2-苯基-1-氧杂-4-氮杂螺[4.5]癸烷,产率分别为54.58%、74.39%、53%、79%、88.52%及66.72%。产物结构进行了红外光谱、1HNMR、13CNMR及元素分析表征;并对Ⅲc物质进行了单晶结构解析。初步的生物测定实验表明,在每kg土含10 mg乙草胺的毒土中,化合物Ⅲc浸种浓度为50μmol/L时玉米株高恢复率达81.92%。
Abstract ：4-Nitro-3-hexanot, 3-nitro-4-heptanol and 2-nitro-l-phenyl-l-propanol were first synthesized from nitroalkane and aldehyde;then they were reduced to 4-amino-3-hexanol, 3-amino-4-heptanol and 2-amino-l-phenyl-l-propanol with iron powder and concentrated HC1. As latent herbicide safener, the six title compounds, including N-dichloroacetyl-2,2,4-trimethyl-1,3-oxazolidine, N-dichloroaeetyl-4- methyl-2-propyl-1, 3-oxazolidine, N-diehloroacetyl-3-methyl-l-oxa-4-aza-spiro [ 4.5 ] decane, N- dichloroacetyl-2,3-diethyl-l-oxa-4-aza-spiro [ 4.5 ] decane, N-dichloroacetyl-3-ethyl-2-propyl-1 -oxa-4- aza-spiro [ 4.5 ] decane and N-dichloroaeetyl-3-methyl-2-phenyl-l-oxa-4-aza-spiro [ 4.5 ] decane, were prepared from amino alcohol, ketone（ or aldehyde） and dichloroaeetyl chloride with triethylamine as acid acceptor in the yield of 54.58% ,74. 39% ,53% ,79% ,88.52% and 66.72% respectively. The structures of the compounds were confirmed by IR,HNMR, 13 CNMR and elemental analysis, and the compound of II1 e was further characterized by means of X-ray diffraction. The preliminary biological test shows that the recovery rates of the plant height could attain 81.92% with 50 μmoL/L of compound Ⅲc when the concentration of acetochlor in the soil was 10 me/k.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第11期1316-1320,共5页
Fine Chemicals
基金
国家自然科学基金项目(30900953)~~
