Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 53353682 | HCID 53353682 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 53353683 | HCID 53353683 | 34.1% |
Reaction Steps
4,5-Dichloro-2-(3,3,5,5-tetramethylcyclohexyl)pyridazin-3-one (0.3 g, 1.475 mmoles) was dissolved in DMSO (20 mL) and a 40% aqueous solution of methylamine (0.6 mL, 1.7 mmoles) was added with stirring. Heated at 100° C. overnight. Allowed to cool and then poured into water. A solid precipitated out and was filtered off. Purified using a silica cartridge eluted with ethyl acetate:isohexane (3:7) to give the product as a cream solid (150 mg). 1H NMR (300 MHz CDCl3) 7.65 (s, 1H), 5.35 (m, 1H), 4.7 (brs, 1H), 3.05 (d, 3H, J=5 Hz), 1.55 (m, 4H), 1.3 (m, 1H), 1.15 (m, 1H), 1.15 (s, 6H), 0.95 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09062004B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-7fdfa777e5164df69e1e6a5e6b50d23b |
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| Source note | uspto-grants-2015_06 |
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