Water → HCID 21427243, compound

HRID 437918Notes

Reaction equation

HRID 437918 reaction equation
O.[C:2](Cl)(=[O:7])[CH2:3][CH2:4][CH2:5][CH3:6].[CH3:9][NH:10][C:11](=[O:29])[CH2:12][NH:13][C:14](=[O:28])[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].CNC(=O)[C@H](CC1C=CC=CC=1)NC(=O)C1C(I)=C(N)C(I)=C(C(O)=O)C=1I>CC(N(C)C)=O>[CH3:9][NH:10][C:11](=[O:29])[CH2:12][NH:13][C:14](=[O:28])[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

6

Reactant 4

HCID 962WaterHCID 61186Valeryl chlorideHCID 21427288HCID 21427288, compoundHCID 54110808HCID 54110808, 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-triiodobenzoyl)-glycine methylamide (IV a), m.p. 252°-253° C. (under decomposition), in 120 ml. of dimethylacetamide. After agitating the reaction mixture overnight at room temperature, 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-e86766cd40094881bf3cb42d2e65e2d2
Source dataset
uspto-grants-1977_06
Patent number
US04032567

Reaction notes

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