Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cesium fluoride → Methyl 2-ethynylbenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cesium fluoride | HCID 25953 | — |
| 반응물 | Methyl 2-((trimethylsilyl)ethynyl)benzoate | HCID 11053512 | — |
| 용매 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 생성물 | Methyl 2-ethynylbenzoate | HCID 373287 | 96.3% |
반응 단계
To a solution of 2-trimethylsilanylethynyl-benzoic acid methyl ester (540 mg, 2.32 mmol) in acetonitrile/water (20 mL/5 mL) is added cesium fluoride (1.41 g, 9.30 mmol). The reaction is stirred at room temperature. After 4 h, the reaction is concentrated and the residue is partitioned between EtOAc (100 mL) and 0.2N HCl (30 mL). The aqueous layer is extracted with EtOAc (100 mL) and the combined organic layers are washed with brine, dried (MgSO4), filtered, and concentrated. The residue is chromatographed eluting with 0 to 5% EtOAc/Hexanes to yield the title compound (358 mg, 96%). GC/MS: 160.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08106077B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-b2bc4d24489c4b2ca44e931528859e18 |
| 출처 메모 | uspto-grants-2012_01 |