Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Pyrosulfite | HCID 656671 | — |
| Reactant | 4-{2-[Methyl(pyridin-2-yl)amino]ethoxy}benzaldehyde | HCID 10422546 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86614376 | HCID 86614376 | 98% |
Reaction Steps
4-[2-(N-methyl-N-(2-pyridyl)amino)ethoxy]benzaldehyde (20 gms, 84% HPLC purity) was stirred with methanol (200 ml) and cooled to 15° C. A solution of sodium metabisulphite (22 gms, 0.115M) in water (40 ml) was added drop wise to the above solution over a time period of about 15 to 20 minutes, whilst maintaining the temperature below about 20° C. The reaction mixture was then cooled to 10° C. and stirred for about 2 hours. The resulting solid precipitate was then filtered and washed with methanol (25 ml) and water (25 ml). The solid was then dried in a vacuum oven at 40° C. to obtain the title compound (20 gms, 98% HPLC purity).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07598387B2 |
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| Source dataset | uspto-grants-2009_10 |
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| ORD ID | ord-c7dca6d9da764c77895c5bcc4733e54d |
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| Source note | uspto-grants-2009_10 |
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