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Acetaldehyde → 5-(Benzoxazol-2-yl)-1-benzyl-2-methylbenzimidazole

HRID 74181
ノート
印刷プレビュー

反応式

HRID 74181 の反応式
[CH2:1]([NH:8][C:9]1[CH:15]=[CH:14][C:13]([C:16]2[O:17][C:18]3[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=3[N:20]=2)=[CH:12][C:10]=1[NH2:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:25](=O)[CH3:26].OOS([O-])=O.[K+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[O:17]1[C:18]2[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=2[N:20]=[C:16]1[C:13]1[CH:14]=[CH:15][C:9]2[N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:25]([CH3:26])=[N:11][C:10]=2[CH:12]=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 4

HCID 177AcetaldehydeHCID 11430Potassium CarbonateHCID 23707502Potassium hydroxy sulfiteHCID 674988042-(2-Benzylaminoanilin-5-yl)benzoxazole

生成物 1

HCID 674982395-(Benzoxazol-2-yl)-1-benzyl-2-methylbenzimidazole収率 41%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 2-(2-benzylaminoanilin-5-yl)benzoxazole (see Working Example 17-2) (80.0 mg, 0.254 mmol) in dimethylformamide (2 mL) was added an aqueous solution of acetaldehyde (approx. 90%, 47.7 μL, 0.761 mmol) and oxone (102 mg, 0.165 mmol), and this was stirred at room temperature for 3 hours. After the reaction was complete, aqueous potassium carbonate solution was added, and this was extracted with ethyl acetate. The organic layer obtained was dried over anhydrous sodium sulfate, filtered, and concentrated to give an oil that was purified by silica gel column chromatography to yield the title compound (35.2 mg, 41% yield) as light brown crystals.

後処理

  1. extractionthis was extracted with ethyl acetate
  2. customThe organic layer obtained
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give an oil that
  7. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-0f77a931e91d4ebeaa08f908fc57f930
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829035B2

反応ノート

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