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Bismuth-oxygen → 1-(3-Methylphenyl)-2-[4-(methylthio)phenyl]ethane-1,2-dione

HRID 2231126
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HRID 2231126 반응식
[OH:1][CH:2]([C:12]1[CH:17]=[CH:16][C:15]([S:18][CH3:19])=[CH:14][CH:13]=1)[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[CH:6]=1)=[O:4].[Bi]=O>C(O)(=O)C>[CH3:11][C:7]1[CH:6]=[C:5]([C:3](=[O:4])[C:2]([C:12]2[CH:13]=[CH:14][C:15]([S:18][CH3:19])=[CH:16][CH:17]=2)=[O:1])[CH:10]=[CH:9][CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6327914Bismuth-oxygen2회HCID 184638162-Hydroxy-1-(3-methylphenyl)-2-[4-(methylthio)phenyl]-ethanone

생성물 1

HCID 184636051-(3-Methylphenyl)-2-[4-(methylthio)phenyl]ethane-1,2-dione수율 43.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
90 °C

실험 절차

The ketone from step 2 (30.5 mmol, 8.31 g) was diluted with acetic acid (90 ml) and heated to ˜90° C. Bi2O3 (30.5 mmol, 14.2 g) was added. After stirring 15 minutes, additional bismuth oxide (15 mmol, 7 g) was added. After 30 additional minutes, the mixture was filtered through silica and Celite®, then lyophilized. The residue was subjected to chromatography (3:1 hexane: ethyl acetate), affording the title compound as a yellow solid (3.56 g, 43%), which was used in the next step.

후처리

  1. filtrationAfter 30 additional minutes, the mixture was filtered through silica and Celite®

출처 및 근거

ORD 기록
ord-9a90ca9d028f4129a8f56a4dc44650dd
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06426360B1

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