HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 66897838, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 86636294 | HCID 86636294 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66897838 | HCID 66897838 | 58% |
Reaction Steps
A solution of 6-chloro-2,4,8,15,22-pentaazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaene bis(trifluoroacetate) (10 mg, 18 μmol) in acetonitrile (0.28 mL) was treated with pyridine (7.3 μL, 91 μmol) followed by acetic anhydride (2.1 μL, 22 μmol) and stirred for 16 h. The reaction mixture was quenched with a few drops of acetic acid and purified by preparative LCMS to give the desired product (5 mg, 58%) as a solid. LCMS for C19H17ClN5O (M+H)+: m/z=366.0. 1H NMR (400 MHz, DMSO-d6): δ 9.61 (s, 1H), 9.24 (s, 1H), 8.16 (s, 1H), 8.06 (dd, J=2.0, 1.8 Hz, 1H), 7.93 (s, 1H), 7.32-7.21 (m, 4H), 7.13 (dd, J=8.2, 1.4 Hz, 1H), 6.97 (dd, J=7.8, 1.2 Hz, 1H), 4.61 (br s, 2H), 1.73 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871753B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-491e6a085f994210b6d37fe325eba24b |
| Source note | uspto-grants-2014_10 |