Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dimethoxyethane → HCID 23365812, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Bis(trimethylsilyl)acetylene | HCID 84564 | — |
| 반응물 | 2-Iodo-4-[(methylsulfonyl)methyl]benzenamine | HCID 19371784 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 23365812 | HCID 23365812 | 83% |
반응 단계
To a solution of 1,2-dimethoxyethane (DME, 70 mL) was added 2 -iodo-4-[(methylsulfonyl)methyl]benzenamine (1) (1.9 g, 0.0061 mol), bis(trimethylsilyl) acetylene (1.56 g, 0.00915 mol), tetrakistriphenylphosphine Pd(O) (0.705 g, 0.00061 mol) and saturated aqueous Na2CO3 (5 mL). The reaction was heated at reflux for 48 h. The solvent was removed in vacuo and the residue was dissolved in EtOAc and washed with brine. The organic layer was dried over MgSO4, filtered and evaporated to give the crude product. Silica gel chromatography (20-100% EtOAc gradient in hexane followed by 5-10% MeOH gradient in EtOAc) of the concentrate afforded the product (2) (1.42 g, 83%) as a brown oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05468768 |
| 출처 데이터셋 | uspto-grants-1995_11 |
| ORD ID | ord-4886fc6c00284f27b3cec637fc1a9d33 |
| 출처 메모 | uspto-grants-1995_11 |