HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → HCID 86636284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| 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 57962578 | HCID 57962578 | — |
| Reactant | HCID 86636286 | HCID 86636286 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Diisopropylethylamine | HCID 81531 | — |
| Product | HCID 86636284 | HCID 86636284 | 12% |
Reaction Steps
A solution of {1-[(5-methylisoxazol-3-yl)carbonyl]piperidin-4-yl}acetic acid (16 mg, 0.063 mmol) (prepared in Example C49, step I), N,N,N′,N′-tetramethyl-O-(7-azabenzotriazol-1-yl)uronium hexafluorophosphate (65 mg, 0.17 mmol) in N,N-dimethylformamide (0.8 mL) and N,N-diisopropylethylamine (26 μL) was stirred for 15 minutes. A solution of 6-fluoro-2,4,8,22-tetraazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-amine bis(trifluoroacetate) (20 mg, 0.06 mmol) in N,N-dimethylformamide (0.3 mL) and was added to the previous solution and stirred overnight. The reaction mixture was purified by preparative HPLC (pH 2) to give the desired product (4 mg, 12%). LCMS for C30H31FN7O3 (M+H)+: m/z=556.2
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871753B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-8549897cfdbf41b58acb44878e00fcd2 |
| Source note | uspto-grants-2014_10 |