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Sodium hydride → 3-[1-(2-Bromomethyl-benzyl)-indol-3-yl]-4-(1-methyl-indol-3-yl)-furan-2,5-dione

HRID 1859198
ノート
印刷プレビュー

反応式

HRID 1859198 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]2[C:11](=[O:26])[O:12][C:13](=[O:25])[C:14]=2[C:15]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:17]([CH3:24])[CH:16]=2)=[CH:2]1.[H-].[Na+].Br[CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[CH2:37][Br:38]>CN(C)C=O>[Br:38][CH2:37][C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][C:31]=1[CH2:30][N:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]2[C:11](=[O:26])[O:12][C:13](=[O:25])[C:14]=2[C:15]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:17]([CH3:24])[CH:16]=2)=[CH:2]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

5

反応物 3

HCID 24758Sodium hydrideHCID 66665o-Bis(bromomethyl)benzeneHCID 148557143-(1-Methyl-indol-3-yl)-4-(indol-3-yl)-furan-2,5-dione

生成物 1

HCID 221232673-[1-(2-Bromomethyl-benzyl)-indol-3-yl]-4-(1-methyl-indol-3-yl)-furan-2,5-dione収率 17.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

A suspension of 3-(indol-3-yl)-4-(1-methyl-indol-3-yl)-furan-2,5-dione (1.0 g, 3 mmol) and sodium hydride (154 mg, 3.5 mmol, 55-60% dispersion in oil) in dimethylformamide (20 mL) was stirred and cooled to 0° C., under a stream of nitrogen. After 35 min the solution was transferred to a dropping funnel and added slowly, over 40 min, to a solution of 1,2-bis-bromomethyl-benzene (3.8 g, 14.5 mmol) in dimethylformamide (6 mL). The resulting solution was stirred for 1 h at room temperature under a stream of nitrogen. The reaction was quenched by adding NaHCO3 (aq), and extracted with ethyl acetate. The organic phase was washed with several portions of water and dried (MgSO4). Evaporation followed by chromatography on silica (ethyl acetate:heptane, 3:7) afforded 270 mg of the desired product.

後処理

  1. stirringThe resulting solution was stirred for 1 h at room temperature under a stream of nitrogen
  2. customThe reaction was quenched
  3. additionby adding NaHCO3 (aq)
  4. extractionextracted with ethyl acetate
  5. washThe organic phase was washed with several portions of water
  6. dry with materialdried (MgSO4)
  7. customEvaporation

出典と根拠

ORDレコード
ord-8157b277b9ec44f4b6e9471f085a20cd
出典データセット
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06153641

反応ノート

読み込み中…

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