Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 4-Bromo-2-(2-chloro-1,1-dimethylethyl)anisole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 4-Bromoanisole | HCID 7730 | — |
| 반응물 | 3-Chloro-2-methyl-1-propene | HCID 11241 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Bromo-2-(2-chloro-1,1-dimethylethyl)anisole | HCID 4605778 | 49.4% |
반응 단계
β-Methallyl chloride (90.5 g, 1.0 mole) was added dropwise to a stirred mixture of p-bromoanisole (200 g, 1.07 mole) and sulphuric acid (34.2 g, 0.35 mole) at 35°-40° C. over about 2 hours. After 21/2 hours at ambient temperature, the mixture was dissolved in dichloromethane, washed with water, aqueous sodium bicarbonate and water again, dried over magnesium sulphate and run down. Distillation of the residue gave a small forerun b.p. about 54° C. at 0.2 mm Hg and a main fraction of 182 g (62%) b.p. 99°-120° C. at 0.15-0.2 mm Hg. Recrystallisation from petroleum ether (b.p. 80°-100° C.) gave 137 g pure title product m.p. 82°-4° C. Reduction in volume of the mother liquors afforded a further 14 g product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04263037 |
| 출처 데이터셋 | uspto-grants-1981_04 |
| ORD ID | ord-d984b1adecf9429c99cf63077136d4a1 |
| 출처 메모 | uspto-grants-1981_04 |