Hydrochloric Acid → HCID 15611980, compound

HRID 703753Notes

Reaction equation

HRID 703753 reaction equation
C[O:2][CH:3](OC)[C:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[C:6]([Cl:11])[C:5]=1[O:12][C:13]1[N:18]=[C:17]([O:19][CH3:20])[CH:16]=[C:15]([O:21][CH3:22])[N:14]=1.O.Cl>C(O)(=O)C>[Cl:11][C:6]1[C:5]([O:12][C:13]2[N:14]=[C:15]([O:21][CH3:22])[CH:16]=[C:17]([O:19][CH3:20])[N:18]=2)=[C:4]([CH:9]=[C:8]([Cl:10])[CH:7]=1)[CH:3]=[O:2]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 962Water2×HCID 15611979HCID 15611979, compound

Product 1

HCID 15611980HCID 15611980, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

3,5-Dichloro-2-(4,6-dimethoxypyrimidin-2-yl)oxy benzaldehyde dimethylacetal (2.1 g) was dissolved in acetic acid (50 ml), and then water (10 ml) and 35% hydrochloric acid (1 ml) were added thereto The mixture was reacted at room temperature for 6 hours. The reaction mixture was poured into water, and extracted with toluene. The extract was washed with a 2% sodium hydroxide aqueous solution, and further washed 3 times with water. The toluene phase was dried, and concentrated under reduced pressure The crystal thus obtained was recrystallized from a mixture of carbontetrachloride and hexane to obtain the above identified compound as a white crystal (1.0 g). (Melting point: 132°-133° C.).

Workup

  1. customThe mixture was reacted at room temperature for 6 hours
  2. extractionextracted with toluene
  3. washThe extract was washed with a 2% sodium hydroxide aqueous solution
  4. washfurther washed 3 times with water
  5. dry with materialThe toluene phase was dried
  6. concentrationconcentrated under reduced pressure The crystal
  7. customthus obtained
  8. customwas recrystallized from a mixture of carbontetrachloride and hexane
  9. customto obtain the

Sources & evidence

ORD record
ord-5e104c008e844124b4d2fd6b9eb706b0
Source dataset
uspto-grants-1991_01
Patent number
US04985066

Reaction notes

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