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

HRID 2379672노트

반응식

HRID 2379672 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-732808f566be4b3d885dd0c948999421
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05364767

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