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Dimethylamine → HCID 58504275、化合物

HRID 2407800
ノート
印刷プレビュー

反応式

HRID 2407800 の反応式
[CH:1]([C:3]1[CH:4]=[C:5]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[CH:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1)=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[CH3:33][NH:34][CH3:35]>O1CCCC1>[CH3:33][N:34]([CH2:1][C:3]1[CH:4]=[C:5]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[CH:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1)[CH3:35]
参加物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 674DimethylamineHCID 4321386Methyl 4-(3-formylphenyl)benzoateHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 58504275HCID 58504275、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of methyl 3′-formylbiphenyl-4-carboxylate (0.338 g) was dissolved in 2 mol/L dimethylamine in tetrahydrofuran (20 mL) and stirred at room temperature for 1 hour. Sodium triacetoxyborohydride (0.895 g) was added. The reaction was stirred at room temperature for 5 days and then partitioned between saturated aqueous sodium bicarbonate and ethyl acetate. The organics were dried over magnesium sulfate and concentrated under reduced pressure to afford the crude material, which was purified by flash column chromatography (eluant: 0-5% methanol/dichloromethane (0.5% triethylamine) to furnish the title compound (0.112 g) having the following physical data.

後処理

  1. stirringThe reaction was stirred at room temperature for 5 days
  2. custompartitioned between saturated aqueous sodium bicarbonate and ethyl acetate
  3. dry with materialThe organics were dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto afford the crude material, which
  6. customwas purified by flash column chromatography (eluant

出典と根拠

ORDレコード
ord-ba722ca47dfa4032884b0c26287b0228
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809538B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート