HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 58138257, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 66919737 | HCID 66919737 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 58138257 | HCID 58138257 | 56.6% |
Reaction Steps
Heat a solution of N-[1-methyl-1-(2-trifluoromethyl-pyrimidin-4-yl)-ethyl]-acetamide (15.4 g, 62 mmol) and aqueous 5N HCl (150 mL) to 100° C. for 20 hours then cool to room temperature. Extract the reaction with diethyl ether (2×) then make the aqueous layer alkaline with aqueous 5N NaOH. Extract the aqueous layer with diethyl ether (3×), dry the combined organic layers over sodium sulfate, filter, and concentrate under reduced pressure to give 1-methyl-1-(2-trifluoromethyl-pyrimidin-4-yl)-ethylamine (7.2 g, 56%) as a brown oil. 1H NMR (400 MHz, CDCl3): δ 8.80 (d, J=5.3 Hz, 1H), 7.68 (d, J=5.3 Hz, 1H), 1.76 (br s, 2H), 1.49 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08420654B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-ba8723eee2c64605a41d0af368d96712 |
| Source note | uspto-grants-2013_04 |