Acetic Acid → HCID 15987642, compound

HRID 68540Notes

Reaction equation

HRID 68540 reaction equation
[C:1]1([N:7]2[C:12](=[O:13])[N:11]([CH3:14])[C:10](=[O:15])C(C#N)=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[C:19]([OH:22])(=[O:21])[CH3:20]>>[C:1]1([N:7]2[C:12](=[O:13])[N:11]([CH3:14])[C:10](=[O:15])[C:20]([C:19]([OH:22])=[O:21])=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 47801582-Phenyl-4-methyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile

Product 1

HCID 15987642HCID 15987642, compoundYield 45.7%

Conditions

Temperature
120 °C

Procedure

Intermediate d (7.6 g, 0.033 mol) was added to a mixed solvent of glacial acetic acid (100 mL) and HCl (72 mL, 0.86 mol). The mixture was warmed up to 120° C. and reacted under reflux for 4 h. The solvent was evaporated off. To the obtained fraction was added water (400 mL). The mixture was filtered by suction and dried to produce a solid (3.7 g) in a yield of 45.7%.

Workup

  1. customreacted
  2. temperatureunder reflux for 4 h
  3. customThe solvent was evaporated off
  4. additionTo the obtained fraction was added water (400 mL)
  5. filtrationThe mixture was filtered by suction
  6. customdried

Sources & evidence

ORD record
ord-b674334b927e4922a96b129f12ed46d7
Source dataset
uspto-grants-2014_09
Patent number
US08822465B2

Reaction notes

Loading…