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Ethanol → HCID 178463174, compound

HRID 1111127
Notes
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Reaction equation

HRID 1111127 reaction equation
[OH:1][C:2]1[N:3]=[N:4][C:5]([OH:10])=[C:6]([Cl:9])[C:7]=1[Cl:8].[OH-].[Na+].[CH2:13](I)[CH3:14].C(O)C>C1C=CC=CC=1.O>[CH2:13]([N:3]1[C:2](=[O:1])[C:7]([Cl:8])=[C:6]([Cl:9])[C:5]([OH:10])=[N:4]1)[CH3:14]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 4

HCID 702EthanolHCID 6340IodoethaneHCID 14798Sodium HydroxideHCID 178518944HCID 178518944, compound

Product 1

HCID 178463174HCID 178463174, compound

Reagents, catalysts & solvents 2

HCID 241BenzeneSolvent
HCID 962
Water
Solvent

Procedure

A mixture comprising 5.00 g of 3,6-dihydroxy-4,5-dichloropyridazine, 2.21 g of sodium hydroxide, 5.60 g of ethyl iodide, 40 ml of ethanol and water, was stirred at a temperature of from 60° to 70° C. for 4 hours. Most ethanol was distilled off under reduced pressure. Then, dilute hydrochrolic acid and chloroform were added to the residue, and the mixture was vigorously shaked. The chloroform layer was separated and washed with water, followed by drying over sodium sulfate. Then, the solvent was distilled off to obtain a light orange solid substance. The solid substance was treated with benzene to obtain 3.56 g of the above identified compound as colorless crystals.

Workup

  1. distillationMost ethanol was distilled off under reduced pressure
  2. additionThen, dilute hydrochrolic acid and chloroform
  3. additionwere added to the residue
  4. customThe chloroform layer was separated
  5. washwashed with water
  6. dry with materialby drying over sodium sulfate
  7. distillationThen, the solvent was distilled off
  8. customto obtain a light orange solid substance
  9. customto obtain 3.56 g of the

Sources & evidence

ORD record
ord-2e75884f616a4c0c9d2a7a3db9ef9133
Source dataset
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04978665

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes