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HCID 13784978, 화합물 → HCID 14126642, 화합물

HRID 329445
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HRID 329445 반응식
[CH3:1][O:2][C:3]([CH:5]([C:7]1[CH:8]=[CH:9][C:10]([S:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:11]([CH2:13][C:14](OC)=[O:15])[CH:12]=1)[CH3:6])=[O:4]>O>[O:15]=[C:14]1[C:24]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[S:18][C:10]2[CH:9]=[CH:8][C:7]([CH:5]([CH3:6])[C:3]([O:2][CH3:1])=[O:4])=[CH:12][C:11]=2[CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 13784978HCID 13784978, 화합물

생성물 1

HCID 14126642HCID 14126642, 화합물수율 89%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 0.5 g of methyl 5-(1-methoxycarbonylethyl)-2-phenylthiophenylacetate [dicarboxylic acid ester] obtained in Example 1-(3) and 5.3 g of polyphosphoric acid (116%) was stirred at a temperature of 60°-80° C. for 6 hours. The mixture was cooled, and to this was added a mixture of ice and water to decompose excessive polyphosphoric acid. The resulting mixture was extracted with ethyl acetate. The organic layer was separated and washed successively with saturated brine solution, aqueous saturated sodium hydrogen carbonate solution and saturated brine solution. The washed extract was dried over anhydrous sodium sulfate. The solvent was distilled off from the dried extract under reduced pressure, and then the residue was recrystallized from a mixture of benzene and hexane to obtain 0.4 g of methyl 2-(10,11-dihydro-10-oxodibenzo[b,f]thiepin-2-yl)propionate (yield 89%), m.p. 81.0°-82.0° C.

후처리

  1. temperatureThe mixture was cooled
  2. additionto this was added
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. customThe organic layer was separated
  5. washwashed successively with saturated brine solution, aqueous saturated sodium hydrogen carbonate solution and saturated brine solution
  6. extractionThe washed extract
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. distillationThe solvent was distilled off from the dried
  9. extractionextract under reduced pressure
  10. customthe residue was recrystallized from a mixture of benzene and hexane

출처 및 근거

ORD 기록
ord-fc800309d0e64155937b8549eeb6bdef
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04891433

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