Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 1-(2-Bromo-5-chlorophenyl)ethanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Bromo-5-chloro-N-methoxy-N-methylbenzamide | HCID 22236546 | — |
| 반응물 | HCID 178418573 | HCID 178418573 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Tetrahydrofuran toluene | HCID 22635083 | — |
| 생성물 | 1-(2-Bromo-5-chlorophenyl)ethanone | HCID 12486617 | — |
반응 단계
Methylmagnesium bromide (4.26 mL of a 1.4M solution in tetrahydrofuran/toluene, 5.97 mmol) was added dropwise to a stirred solution of 2-bromo-5-chloro-N-methoxy-N-methylbenzamide (3-1) (0.554 g, 1.99 mmol) in tetrahydrofuran (20 mL) at approximately 0° C. After 1 h, 1N hydrochloric acid (5 mL) was added and the resulting biphasic mixture was stirred vigorously for about 10 min. The reaction mixture was poured into water and extracted three times with ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. Purification of the crude residue by flash chromatography on silica gel (gradient elution; 0-10% ethyl acetate/hexanes as eluent) provided 3-3 (0.44 g) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06818658B2 |
| 출처 데이터셋 | uspto-grants-2004_11 |
| ORD ID | ord-994732bb6d2942fbb576ed31e579f72d |
| 출처 메모 | uspto-grants-2004_11 |