Ammonium Chloride → 1-methyl-1H-indol-6-amine

HRID 1886952노트

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HRID 1886952 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:11]([O-])=O)[CH:9]=2)[CH:4]=[CH:3]1.[Cl-].[NH4+]>C(O)C.O.[Fe]>[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH2:11])[CH:9]=2)[CH:4]=[CH:3]1

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 106073591-Methyl-6-nitro-1H-indole

생성물 1

HCID 105347991-methyl-1H-indol-6-amine수율 40.2%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 19096565Water ethanol용매

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온도
70 °C

실험 절차

1-methyl-6-nitro-1H-indole (90 mg, 0.51 mmol), ammonium chloride (55 mg, 1.02 mmol) and iron powder (143 mg, 2.55 mmol) were suspended in ethanol/water (2 mL/1 mL) and heated at 70° C. for 2 h. After cooling, the solution was filtrated through a pad of Celite®, which was washed with ethanol. Ethyl acetate was added to the filtrate and the organic layer was washed with water twice. The combined organic layers were dried over anhydrous MgSO4 and evaporated to afford 30 mg (37%) of the title compound

후처리

  1. temperatureAfter cooling
  2. filtrationthe solution was filtrated through a pad of Celite®, which
  3. washwas washed with ethanol
  4. additionEthyl acetate was added to the filtrate
  5. washthe organic layer was washed with water twice
  6. dry with materialThe combined organic layers were dried over anhydrous MgSO4
  7. customevaporated

출처 및 근거

ORD 기록
ord-011eabb246ba4d59aaaa47f6f1982497
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501713B2

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