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Hydrochloric Acid → HCID 178437926、化合物

HRID 2412887
ノート
印刷プレビュー

反応式

HRID 2412887 の反応式
C[O:2][C:3]1[C:4]2[N:5]([C:15]([CH2:18][CH3:19])=[N:16][N:17]=2)[C:6]2[C:11]([N:12]=1)=[CH:10][C:9]([O:13][CH3:14])=[CH:8][CH:7]=2.Cl>C(O)(=O)C>[CH2:18]([C:15]1[N:5]2[C:6]3[C:11]([N:12]=[C:3]([OH:2])[C:4]2=[N:17][N:16]=1)=[CH:10][C:9]([O:13][CH3:14])=[CH:8][CH:7]=3)[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 133856951-Ethyl-4,7-dimethoxy-[1,2,4]triazolo[4,3-a]quinoxaline

生成物 1

HCID 178437926HCID 178437926、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture consisting of 3.3 g. (0.013 mole) of 4,7-dimethoxy-1-ethyl-[1,2,4]triazolo[4,3-a]quinoxaline, 33 ml. of 1N hydrochloric acid and 99 ml. of glacial acetic acid was refluxed for a period of two hours. Upon completion of this step, the reaction mixture was cooled to room temperature and poured over ice/water. The resulting mixture was then stirred for a period of 20 minutes and extracted with ethyl acetate. The latter extract next washed with saturated brine and dried over anhydrous magnisium sulfate. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there was finally obtained a yellowish solid product which was washed with water and air-dried to constant weight to ultimately afford 1.87 g. (67%) of pure 1-ethyl-4-hydroxy-7-methoxy-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. >250° C.

後処理

  1. extractionextracted with ethyl acetate
  2. extractionThe latter extract next
  3. washwashed with saturated brine
  4. dry with materialdried over anhydrous magnisium sulfate
  5. customAfter removal of the drying agent
  6. filtrationby means of filtration
  7. customthe solvent by means of evaporation under reduced pressure, there
  8. customwas finally obtained a yellowish solid product which
  9. washwas washed with water
  10. customair-dried to constant weight to ultimately afford 1.87 g

出典と根拠

ORDレコード
ord-ce28fcc8bf0d4bd3acffe8d4266f290b
出典データセット
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04495187

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート