Potassium Carbonate → HCID 58664770, compound

HRID 2222876Notes

Reaction equation

HRID 2222876 reaction equation
C(=O)([O-])[O-].[K+].[K+].[C:7]([CH2:10][CH2:11][C@@H:12]1[C:17](=[O:18])[NH:16][C:15]2[CH:19]=[C:20]([CH2:23][C@H:24]([NH:30][C:31]([O:33][CH2:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:32])[C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH:21]=[CH:22][C:14]=2[O:13]1)(O)=[O:8].S(O)(O)(=O)=O.[NH2:44][C:45]1[NH:46][CH:47]=[CH:48][N:49]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.O>[CH3:38][C:35]([CH3:36])([CH3:37])[CH2:34][O:33][C:31]([NH:30][C@@H:24]([CH2:23][C:20]1[CH:21]=[CH:22][C:14]2[O:13][C@H:12]([CH2:11][CH2:10][C:7](=[O:8])[NH:44][C:45]3[NH:46][CH:47]=[CH:48][N:49]=3)[C:17](=[O:18])[NH:16][C:15]=2[CH:19]=1)[C:25]([O:27][CH2:28][CH3:29])=[O:26])=[O:32]

Participants

8

Reactant 5

HCID 11430Potassium CarbonateHCID 757711-HydroxybenzotriazoleHCID 135136Bis(2-amino-1H-imidazole) sulphateHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 58664775HCID 58664775, compound

Product 1

HCID 58664770HCID 58664770, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6228DimethylformamideSolvent

Procedure

4.6 g of potassium carbonate are added to a solution of 10 g of 9, 4.4 g of 2-aminoimidazole sulfate, 9.26 g of TBTU and 0.9 g of HOBt in 100 ml of absolute DMF, and the mixture is stirred at 700 under nitrogen for 16 hours. The mixture is cooled to room temperature, poured into 750 ml of cold water, the precipitate is separated off, washed with cold water and dried. The crude product is treated with hot acetonitrile and filtered off after cooling. The residue is recrystallised from ethanol, giving 10.

Workup

  1. customthe precipitate is separated off
  2. washwashed with cold water
  3. customdried
  4. additionThe crude product is treated with hot acetonitrile
  5. filtrationfiltered off
  6. temperatureafter cooling
  7. customThe residue is recrystallised from ethanol

Sources & evidence

ORD record
ord-b9d5eec26f8c4b48bf69455578091ebe
Source dataset
uspto-grants-2008_05
Patent number
US07371854B2

Reaction notes

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