Sulfuric Acid → 1-(6-Chloro-3-hydroxyindol-1-yl)ethanone

HRID 1708338ノート

反応式

HRID 1708338 の反応式
S(=O)(=O)(O)O.[CH3:6][C:7]([N:9]1[C:13]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=2[C:11]([O:19]C(C)=O)=[CH:10]1)=[O:8]>O>[Cl:18][C:15]1[CH:14]=[C:13]2[C:12]([C:11]([OH:19])=[CH:10][N:9]2[C:7](=[O:8])[CH3:6])=[CH:17][CH:16]=1

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 117015591-acetyl-6-chloro-1H-indol-3-yl acetate

生成物 1

HCID 227437681-(6-Chloro-3-hydroxyindol-1-yl)ethanone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 572 ml of concentrated sulfuric acid was added to 63 ml of water with stirring and cooling. When the acid solution was at room temperature, 134 g (0.53M) of 6-chloroindoxyl-1,3-diacetate was added, portionwise, with stirring over a period of one hour keeping the temperature of the solution between 20° to 25° C. After stirring for 30 additional minutes after the addition was complete, the solution was poured onto 2 kg ice. The ice was allowed to melt and the insoluble product was filtered off and washed with cold water. This product was then protected from light and air and dried in a vacuum oven at room temperature. The yield of light yellow solid was 110 gm. This product was very unstable and could not be stored for long period without decomposition. It was used immediately in the next step.

後処理

  1. temperaturecooling
  2. customwas at room temperature
  3. stirringportionwise, with stirring over a period of one hour
  4. custombetween 20° to 25° C
  5. stirringAfter stirring for 30 additional minutes
  6. additionafter the addition
  7. filtrationthe insoluble product was filtered off
  8. washwashed with cold water
  9. customdried in a vacuum oven at room temperature
  10. waitcould not be stored for long period without decomposition

出典と根拠

ORDレコード
ord-988026b750aa4018976caf02d774b41b
出典データセット
uspto-grants-1994_10
特許番号
US05358854

反応ノート

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