تفاعل #1509610

ord-367de10a3cab4b43a995523b367e5bc6

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىis prepared
  2. 2
    تركيزthe reaction medium is concentrated to approximately 2 ml
  3. 3
    أخرىprecipitated from 10 ml of ethanol
  4. 4
    ترشيحThe solid is filtered off
  5. 5
    غسيلwashed with ethanol and diethyl ether
  6. 6
    أخرىpurified on silanized silica RP2, elution

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08926945B2uspto-grants-2015_01