참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | (Phenylthio)acetic acid | HCID 59541 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | 2-Bromo-4'-(methylsulfonyl)acetophenone | HCID 735823 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-Phenylthio-4-(4-(methylsulfonyl)phenyl)-5h-furan-2-one | HCID 10269135 | — |
반응 단계
At 0° C., triethylamine (335 μL) was added to a solution of thiophenoxyacetic acid (161 mg) and 2-bromo-1-(4-(methylsulfonyl)phenyl) ethanone (272 mg, WO 9500501, example 9, Step 1) in 5 mL of acetonitrile and the mixture was stirred at 0° C. for 1 h. The reaction mixture was then cooled to -20° C. and DBU (265 μL) was added. The mixture was stirred for 30 min. at -20° C. and was quenched by addition of 1N HCl. The product was extracted with EtOAc, dried over sodium sulfate and partially purified by silica gel chromatography. The impure product was recrystalized from EtOAc/Hexane to afford the title compound as a solid
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06020343 |
|---|
| 출처 데이터셋 | uspto-grants-2000_02 |
|---|
| ORD ID | ord-a7f933a414fb4257bb076908f26569f6 |
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| 출처 메모 | uspto-grants-2000_02 |
|---|
