Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,1'-Thiocarbonyldiimidazole → HCID 178506355, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| 반응물 | 4-(Trifluoromethoxy)benzene-1,2-diamine | HCID 2773959 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178506355 | HCID 178506355 | 103.5% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08163768B2 |
| 출처 데이터셋 | uspto-grants-2012_04 |
| ORD ID | ord-b2377a823b6743a491300075ff1f4a6b |
| 출처 메모 | uspto-grants-2012_04 |