2-Hydroxy-2-phenylacetohydrazide → HCID 22632809, 화합물

HRID 2416620노트

반응식

HRID 2416620 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 22632809HCID 22632809, 화합물수율 482.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-5fac143e2add4eb0ad22222f0729e001
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825192B1

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