反应 #1509610

ord-367de10a3cab4b43a995523b367e5bc6

反应方程式

CCCCC(C(=O)O)N1CCNCCN(C(CCCC(=O)O)C(=O)O)CCN(C(CCCC(=O)O)C(=O)O)CC1
2-[4,7-bis(1,4-dicarboxybutyl]-1,4,7,10-tetraazacyclododec-1-yl]hexanoic acid
[Na+].[OH-]
NaOH
Cl
HCl
O=C1CC(S(=O)(=O)[O-])C(=O)N1O.[Na+]
sulfo-NHS
CCN=C=NCCCN(C)C
EDCI
NCC(O)CO
3-aminopropane-1,2-diol
O=C(O)CN1CCNCCN(CC(=O)O)CCN(CC(=O)O)CC1
product
O=C(O)CN1CCNCCN(CC(=O)O)CCN(CC(=O)O)CC1
DO3A

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他is prepared
  2. 2
    浓缩the reaction medium is concentrated to approximately 2 ml
  3. 3
    其他precipitated from 10 ml of ethanol
  4. 4
    过滤The solid is filtered off
  5. 5
    洗涤washed with ethanol and diethyl ether
  6. 6
    其他purified on silanized silica RP2, elution

实验过程

A solution containing 0.26 mg of 3-aminopropane-1,2-diol in 6 μl of water is prepared. The pH is adjusted to 6 with HCl. 0.5 mg of gallium complex of 2-[4,7-bis(1,4-dicarboxybutyl]-1,4,7,10-tetraazacyclododec-1-yl]hexanoic acid are added to the above solution. The pH is again adjusted before adding 0.071 mg of sulfo-NHS and 0.062 mg of EDCI. The pH is checked and adjusted to 6 with 2N NaOH. After an overnight period at AT, the reaction medium is concentrated to approximately 2 ml and then precipitated from 10 ml of ethanol. The solid is filtered off, washed with ethanol and diethyl ether, and then purified on silanized silica RP2, elution being carried out with water only. 0.2 mg of product is obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08926945B2uspto-grants-2015_01