Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Fluorene → 2-(9H-fluoren-9-yl)ethane-1-thiol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Fluorene | HCID 6853 | — |
| 반응물 | Thiirane | HCID 9865 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(9H-fluoren-9-yl)ethane-1-thiol | HCID 22407029 | 68.1% |
반응 단계
A solution of fluorene (20.0 g; 120 mmol) in THF (200 mL) was cooled to -40° C. and treated with 48 mL of a 2.5M solution of n-butyllithium in hexanes (120 mmol). After stirring for 15 minutes, a solution of ethylene sulfide (6.5 mL; 109 mmol) in 30 mL of THF was added, and the resulting mixture was stirred at -40° C. for 30 minutes and room temperature for 2 hours. The reaction was quenched by the addition of saturated ammonium chloride, the layers were separated, and the organic phase was washed with 10% HCl, dried and concentrated. The crude product was purified on a flash column, eluting with hexane, to provide 16.8 g (62%) of the product as an oil that recrystallized from hexane as a white solid, mp 38°-40° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05519043 |
| 출처 데이터셋 | uspto-grants-1996_05 |
| ORD ID | ord-d7ae73318a8c4e7c8630bf168d4ff67b |
| 출처 메모 | uspto-grants-1996_05 |