Water → HCID 68492039、化合物

HRID 21252ノート

反応式

HRID 21252 の反応式
C([C:3]1[CH:20]=[CH:19][C:6]([C:7]([NH:9][C:10]([CH3:18])([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH3:11])=[O:8])=[CH:5][C:4]=1[O:21][CH2:22][O:23][CH3:24])=O.[CH:25]([O:30][CH3:31])([O:28][CH3:29])OC.C(=O)([O-])O.[Na+].O>CO.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH3:24][O:23][CH2:22][O:21][C:4]1[CH:5]=[C:6]([CH:19]=[CH:20][C:3]=1[CH:25]([O:28][CH3:29])[O:30][CH3:31])[C:7]([NH:9][C:10]([CH3:18])([C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[CH3:11])=[O:8]

参加物

7

反応物 4

HCID 962WaterHCID 9005Trimethyl orthoformateHCID 516892Sodium BicarbonateHCID 86628293HCID 86628293、化合物

生成物 1

HCID 68492039HCID 68492039、化合物収率 101.4%

試薬・触媒・溶媒 2

HCID 521998p-Toluenesulfonic acid monohydrate触媒HCID 887Methanol溶媒

実験手順

4-Formyl-3-methoxymethoxy-N-(1-methyl-1-phenylethyl)benzamide (3.12 g, 9.53 mmol) was dissolved in methanol (30 mL), and the solution was added with trimethyl orthoformate (2.09 mL, 19.1 mmol) and p-toluenesulfonic acid monohydrate (16.4 mg, 0.0952 mmol), followed by stirring at room temperature for 1 hour. The reaction mixture was added with saturated aqueous sodium hydrogencarbonate solution and water, and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to obtain 3-methoxymethoxy-4-dimethoxymethyl-N-(1-methyl-1-phenylethyl)benzamide (3.61 g, yield 100%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-d7388f43054845a49d70b9d54500919b
出典データセット
uspto-grants-2010_06
特許番号
US07745641B2

反応ノート

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