HCID 21844883, compound → HCID 21844923, compound

HRID 618936Notes

Reaction equation

HRID 618936 reaction equation
[NH2:1][C:2]1[C:3]([I:52])=[C:4]([NH:24][C:25]([NH:27][C:28]2[C:33]([I:34])=[C:32]([C:35]([NH:37][CH2:38][CH:39]([O:45][C:46](=[O:48])[CH3:47])[CH2:40][O:41][C:42](=[O:44])[CH3:43])=[O:36])[C:31]([I:49])=[C:30]([NH2:50])[C:29]=2[I:51])=[O:26])[C:5]([I:23])=[C:6]([C:9]([NH:11][CH2:12][CH:13]([O:19][C:20](=[O:22])[CH3:21])[CH2:14][O:15][C:16](=[O:18])[CH3:17])=[O:10])[C:7]=1[I:8]>C(OCC(Cl)=O)(=O)C>[I:52][C:3]1[C:2]([NH:1][C:39](=[O:45])[CH2:40][O:41][C:42](=[O:44])[CH3:43])=[C:7]([I:8])[C:6]([C:9]([NH:11][CH2:12][CH:13]([O:19][C:20](=[O:22])[CH3:21])[CH2:14][O:15][C:16](=[O:18])[CH3:17])=[O:10])=[C:5]([I:23])[C:4]=1[NH:24][C:25]([NH:27][C:28]1[C:33]([I:34])=[C:32]([C:35]([NH:37][CH2:38][CH:39]([O:45][C:46](=[O:48])[CH3:47])[CH2:40][O:41][C:42](=[O:44])[CH3:43])=[O:36])[C:31]([I:49])=[C:30]([NH:50][C:13](=[O:19])[CH2:14][O:15][C:16](=[O:18])[CH3:17])[C:29]=1[I:51])=[O:26]

Participants

3

Reactant 1

HCID 21844883HCID 21844883, compound

Product 1

HCID 21844923HCID 21844923, compound

Reagents, catalysts & solvents 1

HCID 26297Acetoxyacetyl chlorideSolvent

Procedure

N,N'-bis[3-amino-2,4,6-triiodo-5-(2,3-diacetoxypropylaminocarbonyl)phenyl]urea (1.0 g, 0.71 mmol) was dissolved in acetoxyacetyl chloride (5 ml) and the solution was stirred at ambient temperature for 24 h. After heating to 60° C. for 2.5 h, the solution was evaporated to dryness and the residue was triturated with water (40 ml). The tan-colored precipitate was filtered off, washed again with water (20 ml) and dried. Yield: 0.92 g (81%).

Workup

  1. temperatureAfter heating to 60° C. for 2.5 h
  2. customthe solution was evaporated to dryness
  3. customthe residue was triturated with water (40 ml)
  4. filtrationThe tan-colored precipitate was filtered off
  5. washwashed again with water (20 ml)
  6. customdried

Sources & evidence

ORD record
ord-e6a22aeaaa7c44f8830ff75292047522
Source dataset
uspto-grants-1999_09
Patent number
US05958375

Reaction notes

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