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Sodium hydride → HCID 54152907、化合物

HRID 1768647
ノート
印刷プレビュー

反応式

HRID 1768647 の反応式
[CH3:1][C:2]1[C:10]2[N:9]=[C:8]([CH2:11][CH2:12][CH3:13])[NH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[H-].[Na+].Cl[CH2:17][C:18]1[CH:19]=[CH:20][C:21]2[C:27](=[CH:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])[C:26]3[CH:34]=[CH:35][CH:36]=[CH:37][C:25]=3[CH2:24][O:23][C:22]=2[CH:38]=1>CN(C=O)C.C1(C)C=CC=CC=1>[CH3:1][C:2]1[C:10]2[N:9]=[C:8]([CH2:11][CH2:12][CH3:13])[N:7]([CH2:17][C:18]3[CH:19]=[CH:20][C:21]4[C:27](=[CH:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])[C:26]5[CH:34]=[CH:35][CH:36]=[CH:37][C:25]=5[CH2:24][O:23][C:22]=4[CH:38]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 219956454-Methyl-2-propyl-1H-benzimidazoleHCID 54542434HCID 54542434、化合物

生成物 1

HCID 54152907HCID 54152907、化合物収率 61%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

実験手順

4-Methyl-2-propyl-1H-benzimidazole (464 mg) was dissolved in a mixture of 50 ml of DMF and 80 ml of toluene, and 106.4 mg of sodium hydride (60% oily) was added to the solution under ice cooling, followed by stirring for 30 minutes. To the mixture was added 732 mg of Compound 1-c, and the mixture was heated under reflux for 3 hours. After the solvent was distilled off under reduced pressure, the residue was diluted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [eluent: hexane/ethyl acetate/triethylamine (20/5/1)] to give 629 mg (61%) of the product.

後処理

  1. additionwas added to the solution under ice cooling
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 3 hours
  4. distillationAfter the solvent was distilled off under reduced pressure
  5. additionthe residue was diluted with ethyl acetate
  6. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure
  9. customthe residue was purified by silica gel column chromatography [eluent: hexane/ethyl acetate/triethylamine (20/5/1)]

出典と根拠

ORDレコード
ord-3f31b231969443c583662dc0ae47849f
出典データセット
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05378701

反応ノート

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