HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 58138258, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 66911094 | HCID 66911094 | — |
| Product | HCID 58138258 | HCID 58138258 | 36% |
Reaction Steps
Heat a solution of N-[1-(2-cyclopropyl-pyrimidin-4-yl)-1-methyl-ethyl]-acetamide (4.5 g, 20.5 mmol) and aqueous 5N HCl (125 mL) to 100° C. for 18 hours. Cool the mixture 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-(2-cyclopropyl-pyrimidin-4-yl)-1-methyl-ethylamine (1.3 g, 36%) as a dark yellow oil. 1H NMR (400 MHz, CDCl3): δ 8.45 (d, J=5.6 Hz, 1H), 7.12 (d, J=5.6 Hz, 1H), 2.30 (m, 1H), 1.76 (br s, 2H), 1.41 (s, 6H), 1.09 (m, 2H), 1.02 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08420654B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-62e85c6d840547adb6558293659ee25d |
| Source note | uspto-grants-2013_04 |