Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic acid → [2-Benzothiazolyl][1-[2-(4-fluorophenyl)ethyl]-4-piperidinyl]methanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 4-Fluorophenethyl bromide | HCID 573153 | — |
| 반응물 | 4-(Benzthiazole-2-carbonyl)piperidine | HCID 15237009 | — |
| 촉매 | Benzyltriethylammonium bromide | HCID 165294 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | [2-Benzothiazolyl][1-[2-(4-fluorophenyl)ethyl]-4-piperidinyl]methanone | HCID 15337459 | — |
반응 단계
Mix (2-benzothiazolyl)(4-piperidinyl)methanone.CF3CO2H (1.95 g, 5.43 mmol), 2-(4-fluorophenyl)ethyl bromide (1.70 g, 8.35 mmol), benzyltriethylammonium bromide (149 mg, 0.54 mmol), sodium hydroxide (5 g), water (25 mL) and methylene chloride (25 mL). Stir at room temperature under an argon atmosphere overnight, then heat at reflux overnight. Cool the reaction to room temperature, separate the organic phase and extract the aqueous phase with methylene chloride (50 mL). Combine the organic phases, dry (Na2SO4) and evaporate the solvent in vacuo. Purify by chromatography (20% ethyl acetate/hexane with 2% triethylamine) and recrystallize (hexane) to give the title compound as pale yellow needles; mp 97°-98° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05650416 |
| 출처 데이터셋 | uspto-grants-1997_07 |
| ORD ID | ord-2986c784a7864d1d83e439765f4be730 |
| 출처 메모 | uspto-grants-1997_07 |