HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 2-[(3-chloro-1,2,4-triazin-5-yl)amino]-2-methyl-N-(2,2,2-trifluoroethyl) propanamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 3,5-Dichloro-1,2,4-triazine | HCID 12264933 | — |
| Reactant | 2-Amino-2-methyl-N-(2,2,2-trifluoro-ethyl)-propionamide; hydrochloride | HCID 87773384 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 2-[(3-chloro-1,2,4-triazin-5-yl)amino]-2-methyl-N-(2,2,2-trifluoroethyl) propanamide | HCID 89495477 | — |
Reaction Steps
To a Dioxane (12.0 ml) solution of 3,5-dichloro-1,2,4-triazine I-15a (846 mg, 5.64 mmol) was added 2-amino-2-methyl-N-(2,2,2-trifluoroethyl) propanamide hydrochloride (1,242 mg, 5.64 mmol) followed by diisopropylethylamine (2.96 ml, 16.92 mmol). Dichloromethane (2 mL) was added and the reaction stirred for 2 hours at room temp. The reaction was diluted with dichloromethane and poured into saturated sodium bicarbonate. A precipitate formed. The solid was filtered washed with dichloromethane and then dried under reduced pressure to afford the product I-15 (1.02 g, 60.3%). LRMS (ESI) m/z 297.9 [(M+H)+; calcd for: C9H11ClF3N5O: 298.1].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096598B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-70b6eabfe949404090863454be95e349 |
| Source note | uspto-grants-2015_08 |