Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Azobisisobutyronitrile → 2-(3-(Bromomethyl)-5-methylphenyl)acetic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Azobisisobutyronitrile | HCID 6547 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | 2-(3,5-Dimethylphenyl)acetic acid | HCID 4749495 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-(3-(Bromomethyl)-5-methylphenyl)acetic acid | HCID 58168611 | — |
반응 단계
NBS (3.12 g) was added portionwise over 1 hour to a solution of 2-(3,5-dimethylphenyl)acetic acid (3.6 g) and AIBN (0.015 g) in ethyl acetate (100 mL) at 50° C. under nitrogen. More AIBN (0.015 g) was added and the mixture was heated to reflux for 3 hours. The reaction mixture was washed with 10% aqueous sodium chloride solution (2×200 mL), dried over magnesium sulphate, filtered and evaporated. The crude material was purified by flash silica chromatography using 20% ethyl acetate in isohexane containing 1% acetic acid as solvent. Fractions containing the product were evaporated to dryness to afford a solid which was triturated with cyclohexane (10 mL) to yield the subtitled compound as a white solid. Yield 2.10 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08476265B2 |
| 출처 데이터셋 | uspto-grants-2013_07 |
| ORD ID | ord-f2447fa1d584478fb82909664d6f56d8 |
| 출처 메모 | uspto-grants-2013_07 |