海萝胶 → 1,4,7,10-四氮杂环十二烷-1,4,7-三乙酸

HRID 1422428

反应方程式

HRID 1422428 反应方程式
NCC(O)CO.Cl.[C:8]([CH:11]([N:18]1[CH2:29][CH2:28][N:27]([CH:30]([C:37]([OH:39])=[O:38])CCCC(O)=O)[CH2:26][CH2:25][NH:24][CH2:23][CH2:22][N:21]([CH:40](CCCC)[C:41]([OH:43])=[O:42])[CH2:20][CH2:19]1)CCCC(O)=O)([OH:10])=[O:9].C1C(=O)N(O)C(=O)C1S([O-])(=O)=O.[Na+].CCN=C=NCCCN(C)C.[OH-].[Na+]>O>[CH2:25]1[NH:24][CH2:23][CH2:22][N:21]([CH2:40][C:41]([OH:43])=[O:42])[CH2:20][CH2:19][N:18]([CH2:11][C:8]([OH:10])=[O:9])[CH2:29][CH2:28][N:27]([CH2:30][C:37]([OH:39])=[O:38])[CH2:26]1

参与物

8

反应物 6

HCID 313海萝胶HCID 14798二甲基对苯二胺二盐酸HCID 159081-(3-二甲基氨基丙基)-3-乙基碳二亚胺HCID 735613-氨基-1,2-丙二醇HCID 3520574N-羟基琥珀酰亚胺磺酸钠盐HCID 667390892-[4,7-Bis(1,4-dicarboxybutyl]-1,4,7,10-tetraazacyclododec-1-yl]hexanoic acid

产物 1

HCID 1078301,4,7,10-四氮杂环十二烷-1,4,7-三乙酸

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

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.

后处理

  1. customis prepared
  2. concentrationthe reaction medium is concentrated to approximately 2 ml
  3. customprecipitated from 10 ml of ethanol
  4. filtrationThe solid is filtered off
  5. washwashed with ethanol and diethyl ether
  6. custompurified on silanized silica RP2, elution

来源与证据

ORD记录
ord-367de10a3cab4b43a995523b367e5bc6
来源数据集
uspto-grants-2015_01
专利号
US08926945B2

关联笔记

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