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

HRID 2379672ノート

反応式

HRID 2379672 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 is added to 63 ml of water with stirring and cooling. When the acid solution is at room temperature, 134 g (0.53M) of 6-chloroindoxyl-1,3-diacetate is added, portionwise, with stirring over a period of one hour keeping the temperature of the solution between 20° C. and 25° C. After stirring for 30 additional minutes after the addition is complete, the solution is poured onto 2 kilograms of ice. The ice is allowed to melt and the insoluble product is recovered by filtration and washed with cold water. This product is then protected from light and air and dried in a vacuum oven at room temperature. The yield of light yellow solid is about 110 g. This product is very unstable and may not be stored for long periods without decomposition. It is used immediately in the next step.

後処理

  1. temperaturecooling
  2. customis at room temperature
  3. stirringportionwise, with stirring over a period of one hour
  4. customthe temperature of the solution between 20° C. and 25° C
  5. stirringAfter stirring for 30 additional minutes
  6. additionafter the addition
  7. filtrationthe insoluble product is recovered by filtration
  8. washwashed with cold water
  9. customdried in a vacuum oven at room temperature
  10. waitmay not be stored for long periods without decomposition

出典と根拠

ORDレコード
ord-732808f566be4b3d885dd0c948999421
出典データセット
uspto-grants-1994_11
特許番号
US05364767

反応ノート

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