Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → HCID 18449401, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | tert-Butyl [3-(4-bromo-1,3-thiazol-2-yl)-2-oxo-2,3-dihydro-1H-benzimidazol-1-yl]acetate | HCID 86607786 | — |
| 촉매 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 18449401 | HCID 18449401 | — |
반응 단계
To a suspension of tert-butyl [3-(4-bromo-1,3-thiazol-2-yl)-2-oxo-2,3-dihydro-1H-benzimidazol-1-yl]acetate from Step A (250 mg, 0.609 mmol) and triethylamine (0.850 mL, 6.09 mmol) in MeOH (5 mL) was added bis(triphenylphosphine)palladium (II) chloride (86.0 mg, 0.122 mmol). The reaction mixture was heated at reflux under an atmosphere of carbon monoxide (ca. 1 atm) for 48 h, then partitioned between CHCl3 (20 mL) and saturated aqueous NaHCO3 (5 mL). The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography, eluting with a gradient of hexane:EtOAc—100:0 to 60:40, to give the title compound. MS: m/z=412 (M+23).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08173655B2 |
| 출처 데이터셋 | uspto-grants-2012_05 |
| ORD ID | ord-00e807f4c5c64700ba743aa76f6f13a5 |
| 출처 메모 | uspto-grants-2012_05 |