Carbon Dioxide → 2,5-Thiophenedicarboxylic acid

HRID 462037

반응식

HRID 462037 반응식
[S:1]1[C:5]([C:6]([O-:8])=[O:7])=[CH:4][CH:3]=[C:2]1[C:9]([O-:11])=[O:10].[Na+].[Na+].C(=O)=O.[H][H].[S]>O.[N+]([O-])([O-])=O.[Ag+].[Ag]>[S:1]1[C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=[C:2]1[C:9]([OH:11])=[O:10]

참가 물질

8

반응물 4

HCID 280Carbon DioxideHCID 3085128Disodium thiophene-2,5-dicarboxylateHCID 5362487SulfurHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 202732,5-Thiophenedicarboxylic acid

시약·촉매·용매 3

HCID 23954Silver촉매3회HCID 24470Silver Nitrate촉매HCID 962Water용매2회

반응 조건

온도
350 °C

실험 절차

The di-silver of thiophene-2.5-dicarboxylic acid was prepared in 96 mole % yield by reacting 34.4 grams, 0.2 moles, of disodium thiophene-2,5-dicarboxylate in 500 milliliters of water with 0.4 moles of silver nitrate in 500 milliliters of water, collecting the precipitated silver salt on a filter, followed by washing and drying of the salt. The di-silver salt, 7.75 grams, and 0.02 moles, which decomposes at 315° C, was placed as a thin layer of powdered silver salt along the length of a Vycor reactor tube and heated in a furnace under nitrogen at 350° C for two minutes. Carbon dioxide (CO2) evolved with a sudden puffing up. Combustion of the silver salt subsided with the formation of the polymer and with cessation of evolution of CO2. Heating was stopped and the nitrogen purge was maintained while the tube and contents cooled to room temperature. The calculated loss of CO2 for 0.04 moles CO2 was 1.76 grams. Actual weight loss was 1.95 grams. The resulting carbon-like polymer containing silver analyzed: carbon 15.4%, hydrogen 0.6%, sulfur 4.4%, and silver 79.7%.

후처리

  1. customyield
  2. washby washing
  3. customdrying of the salt
  4. customdecomposes at 315° C
  5. temperatureHeating
  6. customthe nitrogen purge
  7. temperaturewas maintained while the tube and contents
  8. temperaturecooled to room temperature

출처 및 근거

ORD 기록
ord-625707e710834491b773f5e8ac21cf1b
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04065442

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