Potassium Carbonate → HCID 21246134, compound

HRID 2118531Notes

Reaction equation

HRID 2118531 reaction equation
[C:1]([NH:5][CH2:6][CH:7]([OH:23])[CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[N:17]=[N:18][C:19](Cl)=[CH:20][CH:21]=1)([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-:25].[K+].[K+]>Cl>[C:1]([NH:5][CH2:6][CH:7]([OH:23])[CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[CH:21]=[CH:20][C:19](=[O:25])[NH:18][N:17]=1)([CH3:4])([CH3:3])[CH3:2]

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 30190301-(tert-Butylamino)-3-[2-(6-chloropyridazin-3-yl)phenoxy]propan-2-ol

Product 1

HCID 21246134HCID 21246134, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

A stirred solution of 3-[2-(3-t-butylamino-2-hydroxypropoxy)phenyl-6-chloropyridazine (10.0 g, 0.03 mol) in 18% hydrochloric acid (60 ml) was heated under reflux for 8 hours. Potassium carbonate was added to the cold solution to take it to pH 10, and after allowing the mixture to stand for 2 hours the solid was collected by filtration and washed with water to give a crude hydrate (10.35 g). Recrystallisation from ethyl acetate gave 6-[2-(3-t-butylamino-2-hydroxypropoxy)phenyl]-3[2H]-pyridazinone (7.42 g) as a colourless solid, m.p. 161.5°-163.5° C.

Workup

  1. temperatureunder reflux for 8 hours
  2. filtrationthe solid was collected by filtration
  3. washwashed with water
  4. customto give a crude hydrate (10.35 g)
  5. customRecrystallisation from ethyl acetate

Sources & evidence

ORD record
ord-9d2ef9e7bb074e9eadffba1a5e4386d8
Source dataset
uspto-grants-1987_07
Patent number
US04678786

Reaction notes

Loading…