HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butylamine → HCID 70913715, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butylamine | HCID 6385 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Reactant | HCID 70874330 | HCID 70874330 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 70913715 | HCID 70913715 | 30% |
Reaction Steps
A mixture of compound 19 (150 mg, 0.34 mmol), tert-butylamine (36 mg, 0.48 mmol), HATU (207 mg, 0.54 mmol) and DIPEA (146 mg, 1.14 mmol) in DMF (5 mL) was stirred at rt for 20 min, diluted with water and extracted with EA. The organic layer was washed with brine, dried over Na2SO4, concentrated and purified by CC (PE/EA=2/1) to give compound 20 (46 mg, 30%) as a white powder. 1H-NMR (300 MHz, CDCl3) δ: 8.17 (s, 1H), 7.93 (d, 1H, J=1.5 Hz), 7.40 (d, 1H, J=1.5 Hz), 6.61 (s, 1H), 4.70 (d, 2H, J=5.4 Hz), 3.84 (d, 2H, J=6.9 Hz), 2.55 (s, 3H), 1.61 (m, 3H), 1.50 (s, 9H), 1.42 (s, 9H), 1.30-1.38 (m, 3H), 0.97-1.03 (m, 3H), 0.63 (m, 2H). MS Calcd.: 488; MS Found: 489 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946446B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-d4fb036e92564b55a8d92786180d4a8b |
| Source note | uspto-grants-2015_02 |