Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chlorotrimethylsilane → 1,2-Difluoro-3-trimethylsilylbenzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chlorotrimethylsilane | HCID 6397 | — |
| 반응물 | 1,2-Difluorobenzene | HCID 9706 | — |
| 반응물 | tert-Butyl methyl ether | HCID 15413 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1,2-Difluoro-3-trimethylsilylbenzene | HCID 10899371 | — |
반응 단계
625 ml (1 mol) of 1.6 M BuLi are added dropwise at −78° C. to a solution of 114 g (1 mol) of 1,2-difluorobenzene in 1 l of dry tetrahydrofuran. After 1 hour, 140 ml (120 g, 1.1 mol) of trimethylsilyl chloride are slowly added dropwise at −78° C. The mixture is allowed to warm to room temperature overnight, and then 200 ml of methyl tert-butyl ether and 200 ml of water are added. The organic phase is washed with water (2×100 ml) and sat. NaCl (1×100 ml) and dried using magnesium sulfate, and the solvent is removed under reduced pressure. 170 g (91%) of 5 distil over from the residue at from 100 to 102° C./70 mbar.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07183447B2 |
| 출처 데이터셋 | uspto-grants-2007_02 |
| ORD ID | ord-5b4a85235cc44b289503edb92ef623ce |
| 출처 메모 | uspto-grants-2007_02 |