Sodium Hydroxide → 1-(4-Amino-3-benzoylphenyl)ethan-1-one

HRID 1380009ノート

反応式

HRID 1380009 の反応式
[NH2:1][C:2]1[CH:15]=[CH:14][C:13]([C:16]2([CH3:21])OCC[O:17]2)=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].Cl(O)(=O)(=O)=O.[OH-].[Na+]>C(O)C>[C:16]([C:13]1[CH:14]=[CH:15][C:2]([NH2:1])=[C:3]([CH:12]=1)[C:4]([C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)=[O:5])(=[O:17])[CH3:21]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24247Perchloric AcidHCID 21828105[2-Amino-5-(2-methyl-1,3-dioxolan-2-yl)phenyl](phenyl)methanone

生成物 1

HCID 132971931-(4-Amino-3-benzoylphenyl)ethan-1-one収率 93.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Amino-5-(2-methyl-1,3-dioxolan-2-yl)benzophenone (1.0 g, 3.54 m mol) was dissolved in 30 ml absolute ethanol. To this was added 1M perchloric acid (14 ml). The resulting mixture was stirred at room temperature for 18 hrs. The mixture was made basic with 3N sodium hydroxide solution and then extracted with several portions of methylene chloride. The combined methylene chloride extracts were washed with water, dried with anhydrous sodium sulfate, and evaporated to yield a yellow product (0.79 g) of mp. 158°-161° C. A portion of the product was recrystallized from a mixture of methylene chloride and hexane to yield material of mp. 158°-162° C.

後処理

  1. extractionextracted with several portions of methylene chloride
  2. washThe combined methylene chloride extracts were washed with water
  3. dry with materialdried with anhydrous sodium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-2d91091396e343bdb3fc7fa4afa1f9e4
出典データセット
uspto-grants-1986_04
特許番号
US04579679

反応ノート

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