Ammonium Hydroxide → HCID 88278296, compound

HRID 618916Notes

Reaction equation

HRID 618916 reaction equation
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][N:8]1[CH2:19][CH2:18][N:17]([CH2:20][C:21]([OH:23])=[O:22])[CH2:16][CH2:15][N:14]([CH:24]([CH:28]([N:32]2[CH2:43][CH2:42][N:41]([CH2:44][C:45]([OH:47])=[O:46])[CH2:40][CH2:39][N:38]([CH2:48][CH2:49][O:50][CH2:51][CH2:52][O:53][CH3:54])[CH2:37][CH2:36][N:35]([CH2:55][C:56]([OH:58])=[O:57])[CH2:34][CH2:33]2)[C:29]([OH:31])=[O:30])[C:25]([OH:27])=[O:26])[CH2:13][CH2:12][N:11]([CH2:59][C:60]([OH:62])=[O:61])[CH2:10][CH2:9]1.C([O-])(=O)C.[Gd+3:67].C([O-])(=O)C.C([O-])(=O)C.[OH-].[NH4+]>O>[CH3:54][O:53][CH2:52][CH2:51][O:50][CH2:49][CH2:48][N:38]1[CH2:39][CH2:40][N:41]([CH2:44][C:45]([OH:47])=[O:46])[CH2:42][CH2:43][N:32]([CH:28]([CH:24]([N:14]2[CH2:13][CH2:12][N:11]([CH2:59][C:60]([OH:62])=[O:61])[CH2:10][CH2:9][N:8]([CH2:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])[CH2:19][CH2:18][N:17]([CH2:20][C:21]([OH:23])=[O:22])[CH2:16][CH2:15]2)[C:25]([OH:27])=[O:26])[C:29]([OH:31])=[O:30])[CH2:33][CH2:34][N:35]([CH2:55][C:56]([OH:58])=[O:57])[CH2:36][CH2:37]1.[Gd:67].[Gd:67]

Participants

5

Reactant 3

HCID 14923Ammonium HydroxideHCID 159771Acetic acid, gadolinium(3+) salt (3:1)HCID 21844876HCID 21844876, compound

Product 1

HCID 88278296HCID 88278296, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of the compound of Example 15 (300 mg, 0.25 mmol) in DI water (10 mL) is treated with gadolinium acetate (212 mg, 0.52 mmol) at ambient temperature, while the pH is maintained at 5.6-6.0 using 1N ammonium hydroxide solution. When the pH becomes steady, the temperature is elevated to 50° C., and the mixture is stirred for 5 days. The solvent is removed by rotary evaporation, and the residue reconcentrated from DI water (5×200 mL). The crude complex is desalted using preparative HPLC to yield the title compound as a white solid after lyophilization.

Workup

  1. customis elevated to 50° C.
  2. customThe solvent is removed by rotary evaporation

Sources & evidence

ORD record
ord-50f7d1a75e694008b1f1c638c34c20ed
Source dataset
uspto-grants-1999_09
Patent number
US05958373

Reaction notes

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