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Ethanol → HCID 21084112、化合物

HRID 347840
ノート
印刷プレビュー

反応式

HRID 347840 の反応式
[CH3:1][O:2][CH2:3][C:4]1[C:13]([N+:14]([O-])=O)=[C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([Br:12])[N:6]2[N:5]=1.C(O)C.O>[Zn].C(O)(=O)C>[Br:12][C:11]1[N:6]2[N:5]=[C:4]([CH2:3][O:2][CH3:1])[C:13]([NH2:14])=[C:7]2[CH:8]=[CH:9][CH:10]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 702EthanolHCID 962WaterHCID 21084116HCID 21084116、化合物

生成物 1

HCID 21084112HCID 21084112、化合物収率 76.7%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

To a suspension of (7-bromo-3-nitropyrazolo[1,5-a]pyridin-2-yl)methyl methyl ether (540 mg) in a mixed solution of ethanol (10 mL), water (5 mL) and acetic acid (1 mL) was added zinc powder (540 mg), and the reaction mixture was heated and stirred for 30 minutes at 60° C. After filtering off insoluble residue, water was added to the filtrate, extraction was performed with ethyl acetate and the organic extract was washed with saturated aqueous sodium bicarbonate and brine. The obtained organic extract was dried over anhydrous magnesium sulfate and filtered, the solvent was evaporated under reduced pressure, the residue was purified by silica gel column chromatography and 7-bromo-2-(methoxymethyl)pyrazolo[1,5-a]pyridine-3-amine (371 mg) was obtained as a brown oil from the n-hexane:ethyl acetate (2:1) fraction.

後処理

  1. temperaturethe reaction mixture was heated
  2. filtrationAfter filtering off insoluble residue, water
  3. additionwas added to the filtrate, extraction
  4. extractionthe organic extract
  5. washwas washed with saturated aqueous sodium bicarbonate and brine
  6. extractionThe obtained organic extract
  7. dry with materialwas dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customthe solvent was evaporated under reduced pressure
  10. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-50fb1a455dbf4336a5f5b91a46a0ece1
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07176216B2

反応ノート

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