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Chemical Structure| 138168-36-2 Chemical Structure| 138168-36-2

Structure of 138168-36-2

Chemical Structure| 138168-36-2

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Product Details of [ 138168-36-2 ]

CAS No. :138168-36-2
Formula : C18H34N4O9
M.W : 450.48
SMILES Code : O=C(O)CN1CCN(CC(=O)O)CCN(CCN(CC(=O)O)CC1)C(CO)C(O)CO
MDL No. :MFCD32067785

Safety of [ 138168-36-2 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H315-H319
Precautionary Statements:P501-P270-P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P312+P330

Application In Synthesis of [ 138168-36-2 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 138168-36-2 ]

[ 138168-36-2 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 57280-22-5 ]
  • [ 497-19-8 ]
  • [ 112193-77-8 ]
  • [ 138168-36-2 ]
YieldReaction ConditionsOperation in experiment
With sodium hydroxide; chloroacetic acid; In methanol; ethanol; water; butan-1-ol; Example 2a 10-(1-Hydroxymethyl-2,3-dihydroxypropyl)-1,4,7-triscarboxymethyl-1,4,7,10-tetraazacyclododecane 68 g (1.7 mol) of sodium hydroxide is added to 141.1 g (250 mmol) of 1,4,7,10-tetraazacyclododecanetetrasulfate in 600 ml of n-butanol. The mixture is heated and water is azeotropically distilled off. Then, 55.0 g (382 mmol) of 4,4-dimethyl-3,5,8-trioxabicyclo-[5,1,0]-octane is instilled. After completion of the addition, it is refluxed for one hour. Then, it is cooled to room temperature, mixed with 500 ml of water and stirred for 30 minutes. The phases are separated and the butanol phase is evaporated to dryness. The residue is taken up in 600 ml of water and extracted three times with ethyl acetate. The water phase is mixed with 95 g of chloroacetic acid and brought to pH 10. After adding 159 g of Na2 CO3, it is heated to 80 C. and stirred for four hours. Then, 20 g of chloroacetic acid is added, and it is stirred for another twelve hours at 80 C. The reaction mixture is cooled to room temperature, adjusted to pH 0.8 with concentrated hydrochloric acid, heated to 60 C. and stirred for one more hour. Then, it is evaporated to dryness, mixed with 400 ml of a mixture of methanol/ethanol 1:1 and again concentrated by evaporation. This process is repeated, the residue is taken up in 1000 ml of methanol, stirred for 90 minutes at 50 C. and cooled to 0 C. The precipitating potassium chloride is suctioned off and washed twice with methanol. The combined filtrates are evaporated to dryness in a vacuum. The yield of crude product is 176 g. It is now dissolved in 200 ml of deionized water and added on a column with 2.7 l of Amberlite AMB 252c. The column is washed with deionized water until conductivity is no longer to be detected in the elude. Then, the product is eluted with water/ammonia. The substance-containing fractions are combined and evaporated to dryness. 105 g (93% of theory) of 10-(1-hydroxymethyl-2,3-dihydroxy-propyl)-1,4,7-triscarboxymethyl-1,4,7,10-tetraazacyclododecane is obtained. Elementary analysis: Cld: C 47.98 H 7.61 N 12.43 (corrected for water) Fnd: C 47.15 H 7.72 N 12.39 Water content: 9.5%
  • 2
  • 1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid trisodium salt [ No CAS ]
  • [ 57280-22-5 ]
  • [ 138168-36-2 ]
YieldReaction ConditionsOperation in experiment
80% Under nitrogen protection, 19.5 kg of tricarboxylic acid sodium salt intermediate 3 was added to 40 L of isopropanol,8.2 kg of <strong>[57280-22-5]4,4-dimethyl-3,5,8-trioxabicyclo[5.1.0]octane</strong> is added,The reaction was conducted under reflux for 10 hours. After the reaction was completed, 25 kg of concentrated hydrochloric acid was added and the mixture was stirred for 1 hour, then concentrated and filtered to obtain 16.7 kg of compound 4 in a yield of 80%.
 

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