Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
m-Chloroperbenzoic acid → 2,4-Dichloro-1-methanesulfinylmethoxy-benzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 반응물 | 2,4-Dichloro-1-methylsulfanylmethoxy-benzene | HCID 68577897 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,4-Dichloro-1-methanesulfinylmethoxy-benzene | HCID 68577849 | 69% |
반응 단계
To an ice cooled solution of the above crude 2,4-dichloro-1-methylsulfanylmethoxy-benzene (17 g) in DCM (200 mL) was added portion wise m-CPBA (13.8 g, 79.75 mmol) during 30 min. The resulting mixture was allowed to reach room temperature and stirring was continued for 16 hrs. The organic phase was washed with water (2×100 mL), 1N NaOH until pH 6-7, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified on silicagel (10 cm) using first heptane (1 L) followed by EtOAc:heptane (1:1) (1 L) and finally EtOAc as eluents. Pure fractions were collected from the pure EtOAc phase and evaporated in vacuo affording 10.1 g (69%) of 2,4-dichloro-1-methanesulfinylmethoxy-benzene as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08383683B2 |
| 출처 데이터셋 | uspto-grants-2013_02 |
| ORD ID | ord-7a2f96e1b8a347fe90d3fc257d9b83fa |
| 출처 메모 | uspto-grants-2013_02 |