摘要
设计了以α-萘酚为原料,在NaOH催化作用下,经与三光气(BTC)反应,合成了中间体氯甲酸萘酯,再与一甲胺-D3-盐酸盐缩合反应,制得目标产物。合成路线优势在于避免使用剧毒物光气和异氰酸酯,且操作简单,工艺流程短,副产物少,收率可达75%以上,氘标记同位素丰度不稀释。产品经HPLC、IR、MS、1HNMR和13CNMR表征,结果表明:化学纯度>99.5%,氘标记同位素丰度>99.6%。
A novel and mild synthesis method of carbaryl（ methyl-D3 ） was designed using a-naphthol as raw material. The intermediate l-naphthyl/V-methyl carbamate was prepared by a-naphthol and triphosgene under the NaOH as the cata- lyst. The target compound carbaryl-（methyl-D3 ） was obtained by condensation with methylamine-D3-hydrochtoride. Synthe- sis route can avoid the use of highly toxio phosgene isocya-hate, and had the advantages of simple operation, short process, less byproduct. The yield of carbary-（ methyl-D3 ） was more than 75% and deuterium labeled isotope abundance is not diluted. The product was confirmed by HPLC, IB, MS, 1HNMB and 13CNMB. The purity was more than 99.5% and the deuterium enrichment was more than 99.6%.
出处
《化学试剂》
CAS
CSCD
北大核心
2013年第9期845-848,850,共5页
Chemical Reagents
基金
上海市科委基地能力提升专项资助项目(11DZ2210700)
上海化学试剂产业技术创新战略联盟资助项目(11DZ0511700-LMCY-5)
