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HCID 86736134, 화합물 → HCID 20377673, 화합물

HRID 1703488
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HRID 1703488 반응식
[S:1]1[C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH:3]=[C:2]1[C:9]([C:11]1[CH:16]=[CH:15][C:14]([C:17](C)([C:23]([O-])=O)[C:18]([O:20]CC)=[O:19])=[CH:13][CH:12]=1)=[O:10]>[OH-].[Na+].C(O)C.O>[S:1]1[C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH:3]=[C:2]1[C:9]([C:11]1[CH:16]=[CH:15][C:14]([CH:17]([CH3:23])[C:18]([OH:20])=[O:19])=[CH:13][CH:12]=1)=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 86736134HCID 86736134, 화합물

생성물 1

HCID 20377673HCID 20377673, 화합물수율 74.7%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 14798Sodium Hydroxide용매

실험 절차

Ethyl 2-{4-(thieno[2,3-b]thien-2-yl)carbonyl-phenyl}-2-methyl-malonate (16.23 g) is suspended in a mixture of 5% (w/v) aqueous sodium hydroxide solution (90 cc) and ethanol (90 cc), and the suspension is heated at the boiling point for 3 hours. After cooling, the reaction mixture is diluted with distilled water (1000 cc), and then extracted three times with diethyl ether (total 600 cc). The aqueous phase is filtered off, acidified to pH 1 by the addition of a 5N aqueous hydrochloric acid solution and extracted three times with diethyl ether (total 600 cc). The combined ether solutions are washed three times with distilled water (total 300 cc), dried over anhydrous sodium sulphate, decolourizing charcoal (1 g) is added, and the solutions are filtered and evaporated. Crude 2-{4-(thieno[2,3-b]thien-2-yl)carbonyl-phenyl}propionic acid (9.9 g), melting at 150° C., is thus obtained.

후처리

  1. temperaturethe suspension is heated at the boiling point for 3 hours
  2. temperatureAfter cooling
  3. extractionextracted three times with diethyl ether (total 600 cc)
  4. filtrationThe aqueous phase is filtered off
  5. additionacidified to pH 1 by the addition of a 5N aqueous hydrochloric acid solution
  6. extractionextracted three times with diethyl ether (total 600 cc)
  7. washThe combined ether solutions are washed three times with distilled water (total 300 cc)
  8. dry with materialdried over anhydrous sodium sulphate
  9. additionis added
  10. filtrationthe solutions are filtered
  11. customevaporated

출처 및 근거

ORD 기록
ord-b73eae8bf9834cbe8d1b5faa895f042d
출처 데이터셋
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04124596

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