2-Hydroxy-2-phenylacetohydrazide → HCID 22632809、化合物

HRID 2416620ノート

反応式

HRID 2416620 の反応式
[C:1]([NH:11][NH2:12])(=[O:10])[CH:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[OH:3].O.[C:14]1([CH3:24])[CH:19]=[CH:18][C:17](S(O)(=O)=O)=[CH:16][CH:15]=1>CN(C)C=O>[C:14]1([C:24]2[O:3][CH:2]([C:4]3[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=3)[C:1](=[O:10])[NH:11][N:12]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 731262-Hydroxy-2-phenylacetohydrazideHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 22632809HCID 22632809、化合物収率 482.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Mandelic acid hydrazide (1.66 g) and trimethyl o-benzoate (1.82 g) were heated under stirring in dimethyl formamide (30 ml) at 120° C. for 12 hours in the presence of p-toluene sulfonate monohydrate (0.2 g). The solvent was evaporated, and the residue was partitioned between ethyl acetate (150 ml) and water (50 ml). The ethyl acetate layer was washed with water (50 ml×2) and brine (50 ml), and then dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by silica gel chromatography (ethyl acetate/hexane, 1:1), to give the title compound as a white powder (1.28 g, 51%).

後処理

  1. customThe solvent was evaporated
  2. customthe residue was partitioned between ethyl acetate (150 ml) and water (50 ml)
  3. washThe ethyl acetate layer was washed with water (50 ml×2) and brine (50 ml)
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe resulting residue was purified by silica gel chromatography (ethyl acetate/hexane, 1:1)

出典と根拠

ORDレコード
ord-5fac143e2add4eb0ad22222f0729e001
出典データセット
uspto-grants-2004_11
特許番号
US06825192B1

反応ノート

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