Water → HCID 21427243, compound

HRID 1606668Notes

Reaction equation

HRID 1606668 reaction equation
[OH2:1].[C:2](Cl)(=[O:7])[CH2:3][CH2:4][CH2:5][CH3:6].[CH3:9][NH:10][C:11](=[O:28])[CH2:12][NH:13][CH2:14][C:15]1[C:20]([I:21])=[C:19]([NH2:22])[C:18]([I:23])=[C:17]([C:24]([OH:26])=[O:25])[C:16]=1[I:27]>CC(N(C)C)=O>[CH3:9][NH:10][C:11](=[O:28])[CH2:12][NH:13][C:14](=[O:1])[C:15]1[C:20]([I:21])=[C:19]([NH:22][C:2](=[O:7])[CH2:3][CH2:4][CH2:5][CH3:6])[C:18]([I:23])=[C:17]([C:24]([OH:26])=[O:25])[C:16]=1[I:27]

Participants

5

Reactant 3

HCID 962WaterHCID 61186Valeryl chlorideHCID 21544332HCID 21544332, compound

Product 1

HCID 21427243HCID 21427243, compound

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Procedure

Under agitation and water cooling, 31.5 ml. of valeroyl chloride is added dropwise to 45.8 g. (0.073 mole) of N-(3-carboxy-5-amino-2,4,6-triiodobenzyl)-glycine methylamide (Iv a), m.p. 252°-253° C. (under decomposition), in 120 ml. of dimethylacetamide. After agitating the reaction mixture overnight at room temprature, the product is precipitated by adding water; then, the product is vacuum-filtered and purified by dissolving the corresponding sodium salt and separation of the free acid by the addition of a mineral acid.

Workup

  1. customthe product is precipitated
  2. additionby adding water
  3. filtrationthen, the product is vacuum-filtered
  4. custompurified
  5. dissolutionby dissolving
  6. customthe corresponding sodium salt and separation of the free acid
  7. additionby the addition of a mineral acid

Sources & evidence

ORD record
ord-9e75ca29e35848cba0b1d926cff8d214
Source dataset
uspto-grants-1976_04
Patent number
US03953501

Reaction notes

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