HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → 7-Nitro-3,4-dihydro-2H-benzo[b][1,4]thiazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-(2-Chloroethylthio)-4-nitroaniline | HCID 59144098 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 7-Nitro-3,4-dihydro-2H-benzo[b][1,4]thiazine | HCID 20496121 | 94% |
Reaction Steps
To a stirred solution of 2-(2-chloroethylthio)-4-nitroaniline (5.13 g, 22.05 mmol) in DMF (70 mL) was added potassium carbonate (9.14 g, 66.1 mmol), followed by sodium iodide (0.330 g, 2.205 mmol). The resulting suspension was stirred at room temperature overnight. The mixture was then diluted with water, and the resulting crystals were collected by vacuum filtration, giving the desired product (4.06 g, 94%). 1H NMR (DMSO-d6) δ 7.81-7.73 (m, 3H), 6.58 (t, J=9.0 Hz, 1H), 3.65-3.60 (m, 2H), 3.01-2.97 (m, 2H); ESI-MS (m/z, %): 197 (MH+, 100), 180 (99).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08106043B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-beec36693adb436fb38bf96dfbc99768 |
| Source note | uspto-grants-2012_01 |