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Water → HCID 13371549、化合物

HRID 745766
ノート
印刷プレビュー

反応式

HRID 745766 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 24345Iodic acidHCID 12795657HCID 12795657、化合物

生成物 1

HCID 13371549HCID 13371549、化合物収率 289.2%

試薬・触媒・溶媒 2

HCID 807Iodine触媒
HCID 176
Acetic Acid
溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-278be343a5784a428300fb6872fe99bd
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04600715

反応ノート

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