Methyl iodide → 3-(1-Ethyl-5-fluoro-indan-1-yl)-1-methyl-7-nitro-1H-indole

HRID 13701

反応式

HRID 13701 の反応式
[CH2:1]([C:3]1([C:13]2[C:21]3[C:16](=[C:17]([N+:22]([O-:24])=[O:23])[CH:18]=[CH:19][CH:20]=3)[NH:15][CH:14]=2)[C:11]2[C:6](=[CH:7][C:8]([F:12])=[CH:9][CH:10]=2)[CH2:5][CH2:4]1)[CH3:2].[CH3:25][O-].[Na+].IC>CN(C)C=O.CCOCC>[CH2:1]([C:3]1([C:13]2[C:21]3[C:16](=[C:17]([N+:22]([O-:24])=[O:23])[CH:18]=[CH:19][CH:20]=3)[N:15]([CH3:25])[CH:14]=2)[C:11]2[C:6](=[CH:7][C:8]([F:12])=[CH:9][CH:10]=2)[CH2:5][CH2:4]1)[CH3:2]

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 10942334Sodium MethoxideHCID 116095063-(1-Ethyl-5-fluoro-indan-1-yl)-7-nitro-1H-indole

生成物 1

HCID 115736303-(1-Ethyl-5-fluoro-indan-1-yl)-1-methyl-7-nitro-1H-indole収率 95.6%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

Combine 3-(1-ethyl-5-fluoro-indan-1-yl)-7-nitro-1H-indole (0.33 g, 1.02 mmol), sodium methoxide (110 mg, 2.04 mmol), and iodomethane (0.10 ml, 1.53 mmol) in dimethylformamide (5 ml) and stir at room temperature under nitrogen overnight. Dilute with ether, wash with water (2×), dry over sodium sulfate, filter, and concentrate to obtain the title compound as a yellow amorphous solid (0.33 g, 94%). LC-MS m/z 339.1 (M++1).

後処理

  1. washwash with water (2×)
  2. dry with materialdry over sodium sulfate
  3. filtrationfilter
  4. concentrationconcentrate

出典と根拠

ORDレコード
ord-becbe1a517f8420a8d9ed13574665c82
出典データセット
uspto-grants-2010_06
特許番号
US07728150B2

関連ノート

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