HCID 12083981, compound → HCID 9876776, compound

HRID 1251641Notes

Reaction equation

HRID 1251641 reaction equation
C1(C[O:8][C:9](=[O:89])[CH2:10][N:11]2[CH2:22][CH2:21][N:20]([CH2:23][C:24]([N:26]([CH2:47][CH2:48][O:49][C:50](=[O:66])[CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH2:64][CH3:65])[CH2:27][CH2:28][O:29][C:30](=[O:46])[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])=[O:25])[CH2:19][CH2:18][N:17]([CH2:67][C:68]([O:70]CC3C=CC=CC=3)=[O:69])[CH2:16][CH2:15][N:14]([CH2:78][C:79]([O:81]CC3C=CC=CC=3)=[O:80])[CH2:13][CH2:12]2)C=CC=CC=1>CCO.[Pd]>[O:66]=[C:50]([O:49][CH2:48][CH2:47][N:26]([CH2:27][CH2:28][O:29][C:30](=[O:46])[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])[C:24](=[O:25])[CH2:23][N:20]1[CH2:21][CH2:22][N:11]([CH2:10][C:9]([OH:89])=[O:8])[CH2:12][CH2:13][N:14]([CH2:78][C:79]([OH:81])=[O:80])[CH2:15][CH2:16][N:17]([CH2:67][C:68]([OH:70])=[O:69])[CH2:18][CH2:19]1)[CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH2:64][CH3:65]

Participants

4

Reactant 1

HCID 12083981HCID 12083981, compound

Product 1

HCID 9876776HCID 9876776, compoundYield 93%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

10% Pd/C (1.6 g) was added to a solution of 10-[2-[bis[2-[(1-oxohexadecyl)oxy]ethyl]amino]-2-oxoethyl]-1,4,7,10-tetraazacyclo-dodecane-1,4,7-triacetic acid tris(phenylmethyl)ester (16 g; 12.9 mmol) in EtOH (500 mL) and the suspension was stirred for 12 h under hydrogen atmosphere at room temperature. After filtration through a Millipore® filter FT 0.45 μm the solution was evaporated under reduced pressure to give the desired compound. Yield 93%. HPLC: 98% (area %). The 13C-NMR, MS and IR spectra were consistent with the structure.

Workup

  1. filtrationAfter filtration through a Millipore®
  2. filtrationfilter FT 0.45 μm the solution
  3. customwas evaporated under reduced pressure

Sources & evidence

ORD record
ord-6255853758a346d291c1fa81e11fb156
Source dataset
uspto-grants-2002_01
Patent number
US06342598B1

Reaction notes

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