Reaction #1509610

Reaction equation

2-[4,7-bis(1,4-dicarboxybutyl]-1,4,7,10-tetraazacyclododec-1-yl]hexanoic acid

NaOH

HCl

sulfo-NHS

EDCI

3-aminopropane-1,2-diol

→

product

DO3A

Solvents

water

Conditions

Workup

1. 1
   Otheris prepared
2. 2
   Concentrationthe reaction medium is concentrated to approximately 2 ml
3. 3
   Otherprecipitated from 10 ml of ethanol
4. 4
   FiltrationThe solid is filtered off
5. 5
   Washwashed with ethanol and diethyl ether
6. 6
   Otherpurified on silanized silica RP2, elution

Procedure

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.

Source