广州化工
廣州化工
엄주화공
Guangzhou Chemical Industry
2015年
19期
76-78
,共3页
高正华%刘敏%赵广福%方红新%先斌%韦琛鸿%宋迎春
高正華%劉敏%趙廣福%方紅新%先斌%韋琛鴻%宋迎春
고정화%류민%조엄복%방홍신%선빈%위침홍%송영춘
对氯苯肼盐酸盐%一锅法%1-(4-氯苯基)-3-吡唑醇
對氯苯肼鹽痠鹽%一鍋法%1-(4-氯苯基)-3-吡唑醇
대록분정염산염%일과법%1-(4-록분기)-3-필서순
4-chlorophenylhydrazine%on-pot method%1-(4-Chlorophenyl)-3-hydroxypyrazole
1-(4-氯苯基)-3-吡唑醇是一种重要的农药中间体,以对氯苯肼盐酸盐为原料,经过环合,氧化反应一锅法合成1-(4-氯苯基)-3-吡唑醇。本文考察了环合试剂,环合催化剂,环合试剂和氧化催化剂的用量,氧化温度,氧化时间对1-(4-氯苯基)-3-吡唑醇收率的影响。用IR和1 H NMR表征了其结构。在最优条件下,1-(4-氯苯基)-3-吡唑醇合成的总收率为82.4%,该路线简单经济,条件温和,收率高,适合工业化生产。
1-(4-氯苯基)-3-吡唑醇是一種重要的農藥中間體,以對氯苯肼鹽痠鹽為原料,經過環閤,氧化反應一鍋法閤成1-(4-氯苯基)-3-吡唑醇。本文攷察瞭環閤試劑,環閤催化劑,環閤試劑和氧化催化劑的用量,氧化溫度,氧化時間對1-(4-氯苯基)-3-吡唑醇收率的影響。用IR和1 H NMR錶徵瞭其結構。在最優條件下,1-(4-氯苯基)-3-吡唑醇閤成的總收率為82.4%,該路線簡單經濟,條件溫和,收率高,適閤工業化生產。
1-(4-록분기)-3-필서순시일충중요적농약중간체,이대록분정염산염위원료,경과배합,양화반응일과법합성1-(4-록분기)-3-필서순。본문고찰료배합시제,배합최화제,배합시제화양화최화제적용량,양화온도,양화시간대1-(4-록분기)-3-필서순수솔적영향。용IR화1 H NMR표정료기결구。재최우조건하,1-(4-록분기)-3-필서순합성적총수솔위82.4%,해로선간단경제,조건온화,수솔고,괄합공업화생산。
As an important intermediate of pesticides, 1-(4-Chlorophenyl)-3-hydroxypyrazole could be synthesized by the cyclization and oxidation from the raw material 4-chlorophenylhydrazine in on-pot method. The process and the influences of factors on the yield were studied, such as cyclization reagents, cyclization catalyst, the ratio of cyclization reagents and the cyclization catalyst, oxidation temperature and oxidation time. The structure was confirmed by IR and 1H NMR. Under the optimal condition, the total yield was 82. 4% based on 4-chlorophenylhydrazine. The process exhibited mild reaction conditions and high yield, and was suitable for industrial production.