HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1'-Thiocarbonyldiimidazole → HCID 178506355, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| Reactant | 4-(Trifluoromethoxy)benzene-1,2-diamine | HCID 2773959 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178506355 | HCID 178506355 | 103.5% |
Reaction Steps
1,1′-thiocarbonyldiimidazole (1.13 g, 6.25 mmol) is added by portions to a solution of 4-(trifluoromethoxy)-ortho-phenylenediamine (1 g, 5.2 mmol) in 5 ml of tetrahydrofuran and the mixture is stirred at room temperature for 16 hours. The reaction mixture is then concentrated under reduced pressure and the residue is dissolved in 100 ml of ethyl acetate and washed with water (2×30 ml). The organic phase is then dried over MgSO4, filtered and concentrated. The residue is triturated in diisopropylether and pentane and dried under vacuum to yield 1.26 g of 2-mercapto-5-trifluoromethoxy-benzimidazole as a yellow powder. Quantitative yield. Analytical LC/MS (method B): retention time=3.69 min. m/z=235.67 (positive ion mode).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163768B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-b2377a823b6743a491300075ff1f4a6b |
| Source note | uspto-grants-2012_04 |