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

HRID 1886952ノート

反応式

HRID 1886952 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 105347991-methyl-1H-indol-6-amine収率 40.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 19096565Water ethanol溶媒

反応条件

温度
70 °C

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-011eabb246ba4d59aaaa47f6f1982497
出典データセット
uspto-grants-2013_08
特許番号
US08501713B2

反応ノート

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