Sodium hydride → HCID 22123282、化合物

HRID 1859201

反応式

HRID 1859201 の反応式
[H-].[Na+].[CH3:3][N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([C:13]2[C:14](=[O:28])[O:15][C:16](=[O:27])[C:17]=2[C:18]2[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[NH:20][CH:19]=2)=[CH:5]1.Cl[CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[C:33]([CH2:37][Cl:38])[N:32]=1>CN(C)C=O>[Cl:38][CH2:37][C:33]1[N:32]=[C:31]([CH2:30][N:20]2[C:21]3[C:26](=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:18]([C:17]3[C:16](=[O:27])[O:15][C:14](=[O:28])[C:13]=3[C:6]3[C:7]4[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=4)[N:4]([CH3:3])[CH:5]=3)=[CH:19]2)[CH:36]=[CH:35][CH:34]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 3166542,6-Bis(chloromethyl)pyridineHCID 14855714HCID 14855714、化合物

生成物 1

HCID 22123282HCID 22123282、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Sodium hydride (60% dispersion in oil, 42 mg, 1.8 mmol), 3-(1-methyl-indol-3-yl)-4-(indol-3yl)-furan-2,5-dione (236 mg, 0.7 mmol) and dimethylformamide (8 mL) were stirred at room temperature for 1 h. The reaction mixture was cooled with ice and 2,6-bis-chloromethyl-pyridine (520 mg, 3.0 mmol) was added in one portion. Stirring was continued at room temperature for 65 h. The solvent was evaporated and the residue partitioned between ethyl acetate and water. The organic phase was washed with water, dried with MgSO4, filtered and evaporated. Chromatography (ethyl acetate/heptane:50/50) gave the title compound, which was not pure. Further purification by Kugelrohr distillation (oil pump, 150° C.) afforded 156 mg of the sub-title product.

後処理

  1. additionwas added in one portion
  2. customThe solvent was evaporated
  3. customthe residue partitioned between ethyl acetate and water
  4. washThe organic phase was washed with water
  5. dry with materialdried with MgSO4
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-ba4fd500a14940a49b7e82ea7599e65e
出典データセット
uspto-grants-2000_11
特許番号
US06153641

関連ノート

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