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Sodium Hydroxide → HCID 178449230, 화합물

HRID 463784
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HRID 463784 반응식
[OH-].[Na+].S(O)(O)(=O)=O.[CH2:8]([NH:12][C:13]([NH2:15])=[NH:14])[CH:9]([CH3:11])[CH3:10].S([O-])([O-])(=O)=O.[Na+].[Na+].[Cl:23][C:24]1[CH:34]=[CH:33][CH:32]=[C:31]([Cl:35])[C:25]=1[CH:26]=[CH:27][C:28](Cl)=[O:29]>O1CCCC1>[ClH:23].[Cl:23][C:24]1[CH:34]=[CH:33][CH:32]=[C:31]([Cl:35])[C:25]=1[CH:26]=[CH:27][C:28]([NH:14][C:13]([NH:12][CH2:8][CH:9]([CH3:11])[CH3:10])=[NH:15])=[O:29]
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HCID 14798Sodium HydroxideHCID 24436Sodium SulfateHCID 403983-(2,6-Dichlorophenyl)prop-2-enoyl chlorideHCID 178449235Isobutylguanidine sulfate

생성물 1

HCID 178449230HCID 178449230, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture of 7.62 g of a 50% aqueous sodium hydroxide solution, 15.65 g isobutylguanidine sulfate and 120 ml of tetrahydrofuran is stirred for 45 minutes. 12 g of anhydrous sodium sulfate are added to the mixture and stirring continued for 40 minutes. A solution of 2,6-dichlorocinnamoyl chloride (11.22 g) in 40 ml of anhydrous tetrahydrofuran is added dropwise, and the reaction mixture stirred overnight. The yellow reaction mixture is filtered, concentrated in vacuo and the resulting yellow oil partitioned between 100 ml of methylene chloride and 150 ml of H2O. The aqueous layer is extracted with methylene chloride, the combined organic extract dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to a yellow oil. The resulting oil is dissolved in hot acetonitrile/methanol, filtered and evaporated on a hot plate. A white solid is collected, M.P. 178°-180° C.

후처리

  1. stirringstirring
  2. waitcontinued for 40 minutes
  3. stirringthe reaction mixture stirred overnight
  4. filtrationThe yellow reaction mixture is filtered
  5. concentrationconcentrated in vacuo
  6. customthe resulting yellow oil partitioned between 100 ml of methylene chloride and 150 ml of H2O
  7. extractionThe aqueous layer is extracted with methylene chloride
  8. extractionthe combined organic extract
  9. dry with materialdried over anhydrous magnesium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo to a yellow oil
  12. dissolutionThe resulting oil is dissolved in hot acetonitrile/methanol
  13. filtrationfiltered
  14. customevaporated on a hot plate
  15. customA white solid is collected

출처 및 근거

ORD 기록
ord-5a9ac91674c6448ab6ba484d73983a35
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04544670

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