6-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(2-morpholin-4-yl-ethoxy)-pyrimidin-2-yl]-benzyl}-2H-pyridazin-3-one Dihydrogenphosphate → 6-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(2-morpholin-4-yl-ethoxy)-pyrimidin-2-yl]-benzyl}-2H-pyridazin-3-one Dihydrogenphosphate Dihydrate

HRID 2042750Notes

Reaction equation

HRID 2042750 reaction equation
[P:1]([OH:5])([OH:4])([OH:3])=[O:2].[CH3:6][N:7]1[CH:11]=[C:10]([C:12]2[CH:13]=[CH:14][C:15](=[O:40])[N:16]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]4[N:30]=[CH:29][C:28]([O:31][CH2:32][CH2:33][N:34]5[CH2:39][CH2:38][O:37][CH2:36][CH2:35]5)=[CH:27][N:26]=4)[CH:20]=3)[N:17]=2)[CH:9]=[N:8]1>O.C(#N)C>[OH2:2].[OH2:31].[P:1]([OH:5])([OH:4])([OH:3])=[O:2].[CH3:6][N:7]1[CH:11]=[C:10]([C:12]2[CH:13]=[CH:14][C:15](=[O:40])[N:16]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]4[N:30]=[CH:29][C:28]([O:31][CH2:32][CH2:33][N:34]5[CH2:35][CH2:36][O:37][CH2:38][CH2:39]5)=[CH:27][N:26]=4)[CH:20]=3)[N:17]=2)[CH:9]=[N:8]1

Participants

3

Reactant 1

HCID 462360536-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(2-morpholin-4-yl-ethoxy)-pyrimidin-2-yl]-benzyl}-2H-pyridazin-3-one Dihydrogenphosphate

Product 1

HCID 673735616-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(2-morpholin-4-yl-ethoxy)-pyrimidin-2-yl]-benzyl}-2H-pyridazin-3-one Dihydrogenphosphate Dihydrate

Reagents, catalysts & solvents 1

HCID 18373917Acetonitrile--water (1/1)Solvent

Conditions

Temperature
50 °C

Procedure

Approx. 50 mg of 6-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(2-morpholin-4-yl-ethoxy)-pyrimidin-2-yl]-benzyl}-2H-pyridazin-3-one dihydrogenphosphate anhydrate in its crystalline modification A1 were dispersed in approx. 0.15 mL of a binary mixture DI water/acetonitrile (1:1, v/v), and shaken as slurry at 50° C. at 1000 rpm for 7 days. The dispersion was then filtered and resulting crystals were dried at ambient conditions on the filter.

Workup

  1. filtrationThe dispersion was then filtered
  2. customresulting crystals
  3. customwere dried at ambient conditions on the filter

Sources & evidence

ORD record
ord-b28230327f3449bbb922591e00bb6136
Source dataset
uspto-grants-2013_11
Patent number
US08586599B2

Reaction notes

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