Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 6-Methoxy-2,3-dihydro-benzo[1,4]dioxin-5-yl-boronic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Dimethyl Ether | HCID 8254 | — |
| 반응물 | Trimethyl borate | HCID 8470 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 생성물 | 6-Methoxy-2,3-dihydro-benzo[1,4]dioxin-5-yl-boronic acid | HCID 22571892 | 98% |
반응 단계
To a solution of methyl ether X (10.0 g, 60 mmol) in 50 ml THF at −78° C. was added n-butyllithium (36 ml, 90 mmol, 2.5 M in hexanes) was added drop-wise. After 1 h the solution was warmed to rt. After 1 h the solution was cooled to −78° C. and trimethyl borate (13.6 ml, 120 mmol) was added. The solution was warmed to rt. After 16 h the mixture was quenched by the addition of water and resulting mixture was acidified with AcOH and extracted with ethyl acetate. The combined organics were washed with saturated NaHCO3, dried with MgSO4, filtered and concentrated in vacuo. The resulting oil was azeotroped with toluene to afford 6-methoxy-2,3-dihydro-benzo[1,4]dioxin-5-yl-boronic acid (13.72 g, 98%) as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08008313B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-bc080b2e2c92426a83032e54ff395209 |
| 출처 메모 | uspto-grants-2011_08 |