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HCID 19759872, 화합물 → HCID 19759867, 화합물

HRID 1586866
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HRID 1586866 반응식
[S:1]1[C:5]2[S:6](=[O:10])(=[O:9])[CH2:7][CH2:8][C:4]=2[CH:3]=[C:2]1C(O)=O>N1C2C(=CC=CC=2)C=CC=1.C(OCC)(=O)C.[Cu]>[S:6]1(=[O:10])(=[O:9])[C:5]2[S:1][CH:2]=[CH:3][C:4]=2[CH2:8][CH2:7]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 19759872HCID 19759872, 화합물

생성물 1

HCID 19759867HCID 19759867, 화합물수율 95%

시약·촉매·용매 3

HCID 23978Copper촉매HCID 7047Quinoline용매HCID 8857Ethyl Acetate용매

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온도
180 °C

실험 절차

Copper dust (13.4 g. 0.20 mol) was added to a solution of 4,5-dihydrothieno[2,3-b]thiophene-2-carboxylic acid-6,6-dioxide (45 g, 0.20 mol) in quinoline (500 mL) in a reaction vessel fitted with an efficient condenser. The well stirred reaction mixture was heated to 180° C. for 1.5 hours under a nitrogen atmosphere. The dark solution was cooled to room temperature and diluted with ethyl acetate (2 L). The solution was washed with 6N HCl, water, saturated sodium bicarbonate, and saturated brine. The organic phase was dried over magnesium sulfate and treated with decolorizing carbon. Filtration and evaporation of solvent gave the title compound as a solid (33 g, 95%).

후처리

  1. customfitted with an efficient condenser
  2. customreaction mixture
  3. temperatureThe dark solution was cooled to room temperature
  4. washThe solution was washed with 6N HCl, water, saturated sodium bicarbonate, and saturated brine
  5. dry with materialThe organic phase was dried over magnesium sulfate
  6. additiontreated with decolorizing carbon
  7. filtrationFiltration and evaporation of solvent

출처 및 근거

ORD 기록
ord-ed5898c3547d47aabaea662bad97657c
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05216020

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