HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 4-Chloro-6-methyl-1,3,5-triazin-2-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | 2,4-Dichloro-6-methyl-1,3,5-triazine | HCID 16083 | — |
| Product | 4-Chloro-6-methyl-1,3,5-triazin-2-amine | HCID 30591 | 73% |
Reaction Steps
A solution of ammonia, 2.0M methyl alcohol (Aldrich, St. Louis, Mo.) (36.0 mL, 72 mmol) was added dropwise at room temperature (slightly exothermic) to a stirred yellow suspension of 2,4-dichloro-6-methyl-1,3,5-triazine (from Example 7) (2.94 g, 18 mmol) in toluene (20.0 mL, 188 mmol) over 1.5 h. The resulting mixture was stirred for an additional 2.5 h, concentrated and purified (ISCO, DCM to 10% MeOH in DCM) to give the desired product 4-chloro-6-methyl-1,3,5-triazin-2-amine (1.88 g, 73%) as a yellow solid. MS (API-ES) m/z 145 (M+H)+; 1H NMR (CD3OD, 300 MHz) δ 2.32 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772480B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-c7fab7cffc0f497fb354fe1373227861 |
| Source note | uspto-grants-2014_07 |