Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2,3-Methylenedioxyphenyl boronic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Triisopropyl borate | HCID 21531 | — |
| 반응물 | 4-Bromo-1,3-benzodioxole | HCID 2776189 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,3-Methylenedioxyphenyl boronic acid | HCID 4192659 | 69.1% |
반응 단계
nBuLi (2.5M in hexanes, 2.38 mL, 5.97 mmol) was dropwise added to a solution of 4-bromo-1,3-benzodioxole (1 g, 4.97 mmol) and triisopropyl borate (1.49 mL, 6.47 mmol) in 50 mL of dry tetrahydrofuran at −78° C. under argon. The reaction was maintained at that temperature for 3 hours, then warmed up to room temperature and cooled back to 0° C. immediately. The solution was acidified to pH=2 with HCl 2N and neutralized to pH=7 with NaOH 2N, it was then extracted with ethyl acetate (3×25 ml), the organic solution was washed with brine, dried over sodium sulphate and the solvent removed under reduced pressure to yield the title compound (570 mg, 69%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07906530B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-47182cfc45854eaabaf89991df4e4618 |
| 출처 메모 | uspto-grants-2011_03 |