Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 23371667 | HCID 23371667 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23371653 | HCID 23371653 | 82% |
Reaction Steps
To a mixture of 2,4-dichloro-6-indolin-1-yl-1,3,5-triazine (30 g, 112 mM) and methylene chloride (300 ml) at 0° C. was added a 33% solution of methylamine (30 ml) in IMS. The mixture was allowed to attain ambient temperature. After two days the mixture was washed with water. The methylene chloride layer was separated, dried (MgSO4), and the solvent evaporated. The resultant solid was recrystallised from toluene: ethanol (70:30). There was thus obtained 2-chloro-4-indolin-1-yl-6-methylamino-1,3,5-triazine (24 g, 82% yield). m.p 239°-240° C.; NMR: DMSOd6 : 2.75-2.95 (3H, complex, rotamers, NHMe), 3.05-3.2 (2H, t,CH2 --CH2N--), 4.0-4.2 (2H,q,CH2CH2N) (rotamers), 6.9-7.3(3H, complex, aromatic), 7.9-8.1 (1H, broad, aromatic), 8.1-8.4(1H, broad, NH).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05332737 |
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| Source dataset | uspto-grants-1994_07 |
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| ORD ID | ord-44b605123c934007bde0993e6fea732c |
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| Source note | uspto-grants-1994_07 |
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