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1-benzoyl-5-nitro-1H-indole → HCID 9856121、化合物

HRID 1359137
ノート
印刷プレビュー

反応式

HRID 1359137 の反応式
[C:1]([N:9]1[C:17]2[C:12](=[CH:13][C:14]([N+:18]([O-])=O)=[CH:15][CH:16]=2)[CH:11]=[CH:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CO.O1CCCC1.C([O-])=O.[NH4+].[Pd]>[C:1]([N:9]1[C:17]2[C:12](=[CH:13][C:14]([NH2:18])=[CH:15][CH:16]=2)[CH:11]=[CH:10]1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 1

HCID 98350711-benzoyl-5-nitro-1H-indole

生成物 1

HCID 9856121HCID 9856121、化合物収率 56%

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 23938Palladium溶媒HCID 2723923Ammonium formate溶媒

反応条件

温度
30 °C

実験手順

1-benzoyl-5-nitro-1H-indole (50 mg) was dissolved in a mixed solvent with methanol (2 ml) and tetrahydrofuran (2 ml), and ammonium formate of an excess amount and palladium/carbon (10%) of a catalytic amount were added. The reacted solution was stirred at around 30° C. for 30 minutes to complete the reduction, filtered through celite and then, concentrated under reduced pressure. Afterward, the residue was dissolved again in ethylacetate (10 ml), washed with water and brine, dried over anhydrous magnesium sulfate, concentrated under reduced pressure and then, triturated with isooctane and isopropyleter. As a result, the present compound (25 mg, productive yield 56%) was obtained as a solid.

後処理

  1. additionwere added
  2. filtrationfiltered through celite
  3. concentrationconcentrated under reduced pressure
  4. dissolutionAfterward, the residue was dissolved again in ethylacetate (10 ml)
  5. washwashed with water and brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customtriturated with isooctane and isopropyleter
  9. customAs a result, the present compound (25 mg, productive yield 56%) was obtained as a solid

出典と根拠

ORDレコード
ord-419943ebf2e0475d976431e20c35e3fa
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06599929B2

反応ノート

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