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Ammonium Chloride → 7-Fluoro-5-methyl-1H-indole

HRID 2354278
ノート
印刷プレビュー

反応式

HRID 2354278 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH3:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-])=O.[CH:12]([Mg]Br)=[CH2:13].[Cl-].[NH4+]>O1CCCC1>[F:1][C:2]1[CH:3]=[C:4]([CH3:11])[CH:5]=[C:6]2[C:7]=1[NH:8][CH:13]=[CH:12]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 67966Benzene, 2-fluoro-4-methyl-1-nitro-HCID 178418507HCID 178418507、化合物

生成物 1

HCID 218747727-Fluoro-5-methyl-1H-indole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3-fluoro-4-nitrotoluene (3.1 g) in tetra hydrofuran (160 mL) was added vinyl magnesium bromide (1.0 mol/L tetra hydrofuran solution, 60.0 mL) at −40° C., and the mixture was stirred at the same temperature for 1 hour. To the mixture was added a saturated aqueous ammonium chloride solution, and the resulting mixture was stirred at room temperature for 1 hour. The mixture was extracted with diethyl ether. The extract was washed with a saturated aqueous ammonium chloride solution, water and brine successively, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on amino-propylated silica gel (eluent: n-hexane/ethyl acetate=19/1-4/1) to give 7-fluoro-5-methyl-1H-indole (0.96 g). The title compound was prepared in a similar manner to that described in Reference Example 1 using this material instead of 4-methyl-1H-indole.

後処理

  1. stirringthe resulting mixture was stirred at room temperature for 1 hour
  2. extractionThe mixture was extracted with diethyl ether
  3. washThe extract was washed with a saturated aqueous ammonium chloride solution, water and brine successively
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by column chromatography on amino-propylated silica gel (eluent: n-hexane/ethyl acetate=19/1-4/1)

出典と根拠

ORDレコード
ord-3f0f7fbb62f94b1789c54a67b2579b84
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07750145B2

反応ノート

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