Dimethylformamide → HCID 18629187, compound

HRID 1060575Notes

Reaction equation

HRID 1060575 reaction equation
Cl[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13])[N:8]=[C:7]([O:15][CH:16]([CH3:18])[CH3:17])[C:6]([O:19][CH:20]([CH3:22])[CH3:21])=[N:5]2.P([O-])(O)(O)=O.[Na+].[CH3:29][N:30]([CH3:33])C=O>>[O:15]=[C:16]1[CH:18]=[CH:29][N:30]([C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][C:11]=2[N+:12]([O-:14])=[O:13])[N:8]=[C:7]([O:15][CH:16]([CH3:18])[CH3:17])[C:6]([O:19][CH:20]([CH3:22])[CH3:21])=[N:5]3)[CH:33]=[CH:17]1

Participants

4

Reactant 3

HCID 6228DimethylformamideHCID 18629199HCID 18629199, compoundHCID 23672064Monosodium phosphate

Product 1

HCID 18629187HCID 18629187, compound

Conditions

Temperature
125 °C

Procedure

A mixture of 4-hydroxypyridine sodium salt 702 mg, the compound 1.63 g obtained in above described (1), and dried dimethylformamide 3.5 mL was stirred at 125° C. for 3 hr. The resultant mixture was added to an ice-cooled solution of sodium dihydrogen phosphate, then the precipitate was collected by filtration with water. The obtained product was dried and crystallized from acetone to give the title compound (pale brown crystal) 1.02 g.

Workup

  1. filtrationthe precipitate was collected by filtration with water
  2. customThe obtained product was dried
  3. customcrystallized from acetone

Sources & evidence

ORD record
ord-9fc5c098dee2493ba9287ebedbc9e74b
Source dataset
uspto-grants-2003_02
Patent number
US06525054B1

Reaction notes

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