HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 11046378, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,5-Dichloro-4-nitroaniline | HCID 23108 | — |
| Reactant | o-Mercapto-N,N-dimethylbenzamide | HCID 88718 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 11046378 | HCID 11046378 | 75% |
Reaction Steps
A solution of 2.5-dichloro-4-nitro-phenylamine (17) (3.0 g, 14.5 mmol) and 2-mercapto-N,N-dimethyl-benzamide (3.0 g, 16.6 mmol) in DMF (50 mL) was heated to reflux with potassium carbonate (10 g) for 24 h. The mixture was poured into ice water and the precipitate was collected by a filtration. A dark colored solid was recrystalized from petroleum ether/methylene chloride yielded 3.8 g of (18) as a pale yellow powder (75%): IR (cm−1, KBr) 3461, 3376, 3153, 3154, 1627, 1575, 1492, 1135; 1H NMR (200 MHz CDCl3) δ 8.23 (s, 1H), 7.3–7.6 (m, 4H), 6.16 (s, 1H), 4.8 (br s, 2H), 3.37 (s, 3H), 2.86 (s, 3H). Anal. (C15H14ClN3O3S) C, H, N.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07041851B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-907cf24006a04f4cb20febfb67c5dd80 |
| Source note | uspto-grants-2006_05 |