Potassium Phosphate, Tribasic → HCID 24768085, compound

HRID 1774475Notes

Reaction equation

HRID 1774475 reaction equation
[O-]P([O-])([O-])=O.[K+].[K+].[K+].[NH2:9][C:10]1([CH3:30])[CH2:15][CH2:14][N:13]([C:16]2[CH:17]=[C:18]([CH:26]=[C:27](Cl)[N:28]=2)[C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:12][CH2:11]1>>[NH2:9][C:10]1([CH3:30])[CH2:15][CH2:14][N:13]([C:16]2[CH:17]=[C:18]([CH:26]=[CH:27][N:28]=2)[C:19]([O:21][C:22]([CH3:25])([CH3:23])[CH3:24])=[O:20])[CH2:12][CH2:11]1

Participants

3

Reactant 2

HCID 62657Potassium Phosphate, TribasicHCID 24768084HCID 24768084, compound

Product 1

HCID 24768085HCID 24768085, compound

Conditions

Temperature
40 °C

Procedure

To a Parr hydrogenation vessel under a nitrogen atmosphere was charged 5% Pd/Al2O3 (1.02 g, 10 wt % load) and K3PO4 (6.92 g, 1.05 equiv) followed by the 1-methyl-2-pyrrolidinone solution from Example 13 (31.4 g of a 31 wt % solution, 29.9 mmol). The vessel was sealed and sparged with hydrogen and then warmed to 40° C. with shaking. After 4 hours, the vessel was sparged with nitrogen, cooled to ambient temperature and filtered. The catalyst and solids were rinsed with 1-methyl-2-pyrrolidinone (2×10 g). The crude solution was used in the next step.

Workup

  1. customThe vessel was sealed
  2. customsparged with hydrogen
  3. customthe vessel was sparged with nitrogen
  4. temperaturecooled to ambient temperature
  5. filtrationfiltered
  6. washThe catalyst and solids were rinsed with 1-methyl-2-pyrrolidinone (2×10 g)

Sources & evidence

ORD record
ord-e363b825b61d4b469fdd596309f74a4e
Source dataset
uspto-grants-2016_02
Patent number
US09260411B2

Reaction notes

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