Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Iodide → 3-(4-Methoxybenzyloxycarbonyl)-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Methyloxybenzyl chloride | HCID 69993 | — |
| 반응물 | 3-Carboxy-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran | HCID 19795843 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 3-(4-Methoxybenzyloxycarbonyl)-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran | HCID 54528214 | 32.4% |
반응 단계
To a suspension of 50 mg (0.163 mmol) of the compound of Example 112 in 0.2 ml of chloroform were added 30.7 mg (0.196 mmol) of p-methoxybenzyl chloride, 16.5 mg (0.163 mmol) of triethylamine and 29.4 mg (0.196 mmol) of sodium iodide, and the mixture was stirred for 5 hours at room temperature, which was poured into ice-water and extracted with dichloromethane. The organic layer was washed with water and with saturated saline solution, dried over anhydrous sodium sulfate and concentrated. The residue was purified by means of silica gel column chromatography (CHCl3) to obtain 22.5 mg (0.0528 mmol) of title compound (yield 32%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05244892 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-650824152b5742c386e87f846affa28e |
| 출처 메모 | uspto-grants-1993_09 |