HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22961855, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Tetrafluoro-m-phenylenediamine dihydrochloride | HCID 149026 | — |
| Reactant | Ether hydrochloride | HCID 10953452 | — |
| Reactant | HCID 22961820 | HCID 22961820 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 22961855 | HCID 22961855 | 99% |
Reaction Steps
The product of step 159a (0.23 g, 0.70 mmol) was deprotected and isolated as the free base in 99% yield according to the procedure of Example 20b, followed by conversion to the dihydrochloride with excess HCl/Et2O. [α]D23 +12.46 (c 0.1, MeOH); 1H NMR (D2O, 300 MHz) δ2.65-2.75 (m, 2H), 3.66 (s, 3H), 4.08-4.19 (m, 2H), 4.43 (s, 2H), 4.53-4.69 (m, 2H), 4.90 (m, 1H), 8.22 (s, 1H), 8.44 (s, 1H), 8.63 (d, J=3.0 Hz, 1H); MS (CI/NH3) m/z 252 (M+H)+. Anal. Calcd for C12H17N3O·2.5 HCl·1.5 H2O·0.4 Et2O: C, 40.93; H, 6.69; N, 10.53. Found: C, 40.96; H, 6.63; N, 10.46.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06127386 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-5ffb49c717364da9a2339963dff0675f |
| Source note | uspto-grants-2000_10 |