反応 #470377

ord-9c57dc03620d4654bfc3504b55ad2625

反応方程式

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
収率 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
収率 81.3%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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%).

出典

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