反应 #470377

ord-9c57dc03620d4654bfc3504b55ad2625

反应方程式

C1CNCCNCCNCCN1
cyclen
O=C(OCc1ccccc1)C(Br)CCCN1C(=O)c2ccccc2C1=O
2-bromo-5-(1,3-dioxo-1,3-dihydroisoindol-2-yl)pentanoic acid benzyl ester
O=C(OCc1ccccc1)C(CCCN1C(=O)c2ccccc2C1=O)N1CCNCCNCCNCC1
product
收率 81.3%
O=C(OCc1ccccc1)C(CCCN1C(=O)c2ccccc2C1=O)N1CCNCCNCCNCC1
5-(1,3-dioxo-1,3-dihydroisoindol-2-yl)-2-(1,4,7,10-tetraazacyclododec-1-yl)pentanoic acid benzyl ester
收率 81.3%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONare added dropwise
  2. 2
    过滤The precipitate is filtered off
  3. 3
    洗涤washed thoroughly with acetonitrile

实验过程

55 g of cyclen base (320 mmol) are dissolved in 550 ml of CH3CN, to which 119.8 g of brominated derivative (2-bromo-5-(1,3-dioxo-1,3-dihydroisoindol-2-yl)pentanoic acid benzyl ester, 288 mmol) dissolved in 550 ml of CH3CN are added dropwise. The medium is stirred at ambient temperature overnight. The precipitate is filtered off and washed thoroughly with acetonitrile. 138 g of product are obtained in the form of a white powder (corrected yield 81.3%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08367039B2uspto-grants-2013_02