Glyoxal → 1-Benzyl-3-(naphthalen-2-yl)-1H-pyrazolo[3,4-b]pyrazine

HRID 34068

反応式

HRID 34068 の反応式
[CH2:1]([N:8]1[C:12]([NH2:13])=[C:11]([NH2:14])[C:10]([C:15]2[CH:24]=[CH:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH:16]=2)=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:25]([CH:27]=O)=O>CO>[CH2:1]([N:8]1[C:12]2=[N:13][CH:25]=[CH:27][N:14]=[C:11]2[C:10]([C:15]2[CH:24]=[CH:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH:16]=2)=[N:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 7860GlyoxalHCID 230701962-benzyl-5-(naphthalen-2-yl)-2H-pyrazole-3,4-diamine

生成物 1

HCID 597972851-Benzyl-3-(naphthalen-2-yl)-1H-pyrazolo[3,4-b]pyrazine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

190 mg of 2-benzyl-5-(naphthalen-2-yl)-2H-pyrazole-3,4-diamine was dissolved in 10 mL of methanol, added with 100 μl of 40% glyoxal aqueous solution, and stirred at room temperature for 5 hours. The reaction solution was partitioned between water and ethyl acetate, and the organic layer was extracted and washed with water. The organic layer was dried over magnesium sulfate, the solvent was evaporated, and the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5), to afford 180 mg of the title compound as a pale yellow powder.

後処理

  1. customThe reaction solution was partitioned between water and ethyl acetate
  2. extractionthe organic layer was extracted
  3. washwashed with water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customthe solvent was evaporated
  6. customthe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5)

出典と根拠

ORDレコード
ord-2a5fe7c910be4257badd2215126efe90
出典データセット
uspto-grants-2008_09
特許番号
US07429609B2

関連ノート

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