广东化工
廣東化工
엄동화공
GUANGDONG CHEMICAL INDUSTRY
2012年
4期
65-66
,共2页
王伟%林勇%俞阳晨%张胜建%张洪
王偉%林勇%俞暘晨%張勝建%張洪
왕위%림용%유양신%장성건%장홍
O-2-氟苯甲基羟胺盐酸盐%丙酮肟%邻氟氯苄%DMSO%[Bmim]OH
O-2-氟苯甲基羥胺鹽痠鹽%丙酮肟%鄰氟氯芐%DMSO%[Bmim]OH
O-2-불분갑기간알염산염%병동우%린불록변%DMSO%[Bmim]OH
O-2-fluorophenyl methyl hydroxylamine hydrochloride%acetone oxime%1-(chloromethyl)-2-fluorobenzene%DMSO%[Bmim]OH
以丙酮肟和邻氟氯苄为原料合成了O-2-氟苯甲基丙酮肟醚,再用盐酸水解得到了O-2-氟苯甲基羟胺盐酸盐。文章系统研究了反应温度、不同溶剂、溶剂含水量等各种实验因素对O-2-氟苯甲基丙酮肟醚的影响,研究了盐酸浓度、水解温度等因素对O-2-氟苯甲基丙酮肟醚水解工艺的影响。两步收率最高分别为92.3%和87.3%。并用核磁等对产品及中间体进行了表征。
以丙酮肟和鄰氟氯芐為原料閤成瞭O-2-氟苯甲基丙酮肟醚,再用鹽痠水解得到瞭O-2-氟苯甲基羥胺鹽痠鹽。文章繫統研究瞭反應溫度、不同溶劑、溶劑含水量等各種實驗因素對O-2-氟苯甲基丙酮肟醚的影響,研究瞭鹽痠濃度、水解溫度等因素對O-2-氟苯甲基丙酮肟醚水解工藝的影響。兩步收率最高分彆為92.3%和87.3%。併用覈磁等對產品及中間體進行瞭錶徵。
이병동우화린불록변위원료합성료O-2-불분갑기병동우미,재용염산수해득도료O-2-불분갑기간알염산염。문장계통연구료반응온도、불동용제、용제함수량등각충실험인소대O-2-불분갑기병동우미적영향,연구료염산농도、수해온도등인소대O-2-불분갑기병동우미수해공예적영향。량보수솔최고분별위92.3%화87.3%。병용핵자등대산품급중간체진행료표정。
The Paper studies the synthetic process of O-2-fluorophenyl methyl hydroxylamine hydrochloride through O-alkylation and hydrolysis from acetone oxime and 1-(chloromethyl)-2-fluorobenzene.The effect of different conditions,such as reaction temperature,solvents,water on the O-alkylation of acetone oxime with 1-(chloromethyl)-2-fluorobenzene,and the temperature,the concentration of HCl,the material ratio on the hydrolysis reaction are studied.The results shown: the yield of O-alkylation is 92.3 % and hydrolysis was 87.3 %.The product and intermediate were characterized by 1H NMR and 13C NMR.