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Water → HCID 13371549, 화합물

HRID 745766
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HRID 745766 반응식
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH3:19])=[CH:15][CH:14]=[CH:13][CH:12]=3)=[O:5])[CH3:2].O.S(=O)(=O)(O)O.[I:26](O)(=O)=O>C(O)(=O)C.II>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH3:19])=[CH:15][C:14]([I:26])=[CH:13][CH:12]=3)=[O:5])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 24345Iodic acidHCID 12795657HCID 12795657, 화합물

생성물 1

HCID 13371549HCID 13371549, 화합물수율 289.2%

시약·촉매·용매 2

HCID 807Iodine촉매
HCID 176
Acetic Acid
용매

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온도
80 °C

실험 절차

5.08 g of 4-methyl-β-carboline-3-carboxylic acid ethyl ester is dissolved in 40 ml of glacial acetic acid and combined with 0.96 ml of water, 0.24 ml of concentrated sulfuric acid, 688 mg of iodic acid, and 1.768 mg of iodine. The mixture is heated to 80° C. for 3 hours. After cooling, the mixture is suctioned off from undissolved material, and the filtrate is evaporated. The residue is taken up in ethanol/water. The thus-formed crystals are suctioned off, taken up in 500 ml of ethyl acetate, and extracted by stirring with 200 ml of 1N sodium hydroxide solution for 15 minutes. The organic phase is separated, concentrated by evaporation, the residue is extracted by stirring in ethyl acetate, and vacuum-filtered, thus obtaining 4.3 g of 6-iodo-4-methyl-β-carboline-3-carboxylic acid ethyl ester, mp 250°-255° C.

후처리

  1. temperatureAfter cooling
  2. customthe filtrate is evaporated
  3. extractionextracted
  4. customThe organic phase is separated
  5. concentrationconcentrated by evaporation
  6. extractionthe residue is extracted
  7. stirringby stirring in ethyl acetate
  8. filtrationvacuum-filtered

출처 및 근거

ORD 기록
ord-278be343a5784a428300fb6872fe99bd
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04600715

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