Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanolamine | HCID 700 | — |
| Reactant | HCID 178426078 | HCID 178426078 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 20040899 | HCID 20040899 | — |
Reaction Steps
A solution of 7-chloro-5-methyl-3-phenyl-1H-pyrazolo[4,3-b]pyridine (D9) (0.63 g) in xylene (15 ml) with ethanolamine (1.5 ml) was heated at reflux for 3 days under nitrogen. The solvent was then removed under reduced pressure and the residue dissolved in water with the minimum amount of methanol with warming. This solution was brought to pH9 by addition of 10% sodium hydroxide and then further diluted with water. The resulting emulsion was left to stand overnight to give the title compound as a pale yellow crystalline solid which was collected, washed with water and dried under vacuum to afford the title compound (0.686 g, 95%), m.p. softening and partial melting at 135° with resolidification and melting at 186°-188°. (Found: C, 64.58; H, 6.42; N, 20.06. C15H16N4O.1/2H2O requires C, 64.96; H, 6.18; N, 20.20%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04833136 |
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| Source dataset | uspto-grants-1989_05 |
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| ORD ID | ord-de5705df418f43568323da8d08ac3cbe |
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| Source note | uspto-grants-1989_05 |
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