Acetic Acid → HCID 178517880, compound

HRID 1477678Notes

Reaction equation

HRID 1477678 reaction equation
[C:1]([OH:4])(=O)C.ClC1[N:11]=[C:10]([N:12]2[CH2:17][CH2:16][C:15]([C:18]3[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=3)=[CH:14][CH2:13]2)[N:9]=[CH:8][N:7]=1.C([O-])(=O)C.[Na+]>O>[F:24][C:21]1[CH:20]=[CH:19][C:18]([C:15]2[CH2:16][CH2:17][N:12]([C:10]3[N:9]=[CH:8][NH:7][C:1](=[O:4])[N:11]=3)[CH2:13][CH:14]=2)=[CH:23][CH:22]=1

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 1178392512-Chloro-4-[4-(4-fluorophenyl)-5,6-dihydropyridin-1(2H)-yl]-1,3,5-triazine

Product 1

HCID 178517880HCID 178517880, compoundYield 89%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
0 °C

Procedure

To an acetic acid (9.0 mL)-water (1.8 mL) solution of 2-chloro-4-[4-(4-fluorophenyl)-5,6-dihydropyridin-1(2H)-yl]-1,3,5-triazine (900 mg, 3.10 mmol) synthesized in Reference Synthesis Example 341, sodium acetate (900 mg, 11.0 mmol) was added and the resultant mixture was stirred at 90° C. for 1 hour. After completion of the reaction, the reaction solution was concentrated under reduced pressure and water was added to the obtained residue, followed by stirring the resultant mixture at 0° C. The precipitated solid was collected by filtration and the solid was dried under reduced pressure to obtain the title compound (750 mg, yield 89%).

Workup

  1. additionwas added
  2. customAfter completion of the reaction
  3. concentrationthe reaction solution was concentrated under reduced pressure and water
  4. additionwas added to the obtained residue
  5. filtrationThe precipitated solid was collected by filtration
  6. customthe solid was dried under reduced pressure

Sources & evidence

ORD record
ord-dd84de5f16aa402182281edc55d48a15
Source dataset
uspto-grants-2016_08
Patent number
US09403798B2

Reaction notes

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