HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 5-Methyl-8-thia-4,6-diazatricyclo[7.4.0.0,2,7]trideca-1(9),2(7),5-trien-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Ethyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate | HCID 78262 | — |
| Product | 5-Methyl-8-thia-4,6-diazatricyclo[7.4.0.0,2,7]trideca-1(9),2(7),5-trien-3-one | HCID 209395 | 62% |
Reaction Steps
To a 25 ml flask was added 4 (225 mg, 1 mmol) and 10 ml CH3CN. HCl gas was passed through the solution for 3 h, before the solvent was evaporated under reduced pressure. The residue was dissolved in 10 mL distilled water and treated with ammonia water solution to generate a white precipitate. The precipitate was collected by filtration to afford 143 mg (62%) of 5 as a white solid: 1H NMR (DMSO-d6) δ 1.75 (m, 4H), 2.48 (s, 3H), 2.69 (m, 2H), 2.83 (m, 2H), 12.16 (s, 1H). Anal. (C11H12N2OS) m/z (ESI) 220.067811 [M]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07982035B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-873b8fb5bcc44adfa7f54f34ff62c7c3 |
| Source note | uspto-grants-2011_07 |