HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → HCID 66604454, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| 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 66604725 | HCID 66604725 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66604454 | HCID 66604454 | — |
Reaction Steps
A mixture of 4-carbamoyl-2-(3-chloro-4-fluorophenyl)-5H-pyrido[3,2-b]indole-7-carboxylic acid 431D (55 mg, 0.143 mmol), 1-methylpiperazine (0.032 mL, 0.287 mmol), N,N-diisopropylethylamine (0.075 mL, 0.430 mmol) and HATU (109 mg, 0.287 mmol) in DMF (1 mL) was stirred for overnight. The mixture was concentrated and purified using preparative HPLC to give titled product. MS (ESI) m/z 466.16 (M+H)+. 1H NMR (DMSO-d6) δ ppm 11.82 (s, 1H), 8.62 (s, 1H), 8.53 (s, 1H), 8.50 (dd, 1H, J=7.1, 2.1), 8.34 (m, 2H), 7.99 (s, 1H), 7.79 (s, 1H), 7.62 (t, 1H, J=8.8), 7.28(d, 1H, J=8.0), 3.67 (bs, 4H), 2.37 (bs, 4H), 2.22 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815840B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-294998bb8a114e89bfdc4e4022636b4f |
| Source note | uspto-grants-2014_08 |