Sulfuric Acid → HCID 19097339, 화합물

HRID 486061노트

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HRID 486061 반응식
Cl.[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10]N)=[CH:6][CH:5]=1.[CH3:12][CH2:13][CH2:14][C:15](=O)[CH2:16][CH2:17][CH3:18].S(=O)(=O)(O)O.C(=O)(O)[O-].[Na+]>C(O)C>[CH2:13]([C:14]1[C:8]2[C:7](=[CH:6][CH:5]=[C:4]([O:3][CH3:2])[CH:9]=2)[NH:10][C:15]=1[CH2:16][CH2:17][CH3:18])[CH3:12]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 312464-HeptanoneHCID 516892Sodium BicarbonateHCID 27239044-Methoxyphenylhydrazine hydrochloride

생성물 1

HCID 19097339HCID 19097339, 화합물수율 87.2%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
10 °C

실험 절차

A mixture of 4-methoxyphenyl hydrazine hydrochloride (3.0 g), 4-heptanone (1.94 g), and sulfuric acid (1.3 ml) in ethanol (10 ml) was stirred at 10° C. for 3 hours. The cooled mixture was poured into aqueous sodium bicarbonate solution, such that the pH was adjusted to 9. The solution was extracted with ethyl acetate, the organic layer separated, washed with water, dried over magnesium sulfate, and concentrated in vacuo. The crude product was chromatographed on silica gel using 25%-ethyl acetate in n-hexanes as eluent to yield 3-ethyl-5-methoxy-2-propylindole (3.22 g).

후처리

  1. extractionThe solution was extracted with ethyl acetate
  2. customthe organic layer separated
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe crude product was chromatographed on silica gel using 25%-ethyl acetate in n-hexanes as eluent

출처 및 근거

ORD 기록
ord-caf00ededb83482591a24e4f44f6c9c3
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05290788

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