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Aniline → HCID 9816404、化合物

HRID 1153731
ノート
印刷プレビュー

反応式

HRID 1153731 の反応式
[N:1]1[C:10]2[C:9](=[O:11])[CH:8]=[CH:7][C:6](=[O:12])[C:5]=2[N:4]=[CH:3][CH:2]=1.[NH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(O)C>[NH:13]([C:8]1[C:9](=[O:11])[C:10]2[N:1]=[CH:2][CH:3]=[N:4][C:5]=2[C:6](=[O:12])[CH:7]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
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 6115AnilineHCID 113556455,8-Quinoxalinedione

生成物 1

HCID 9816404HCID 9816404、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Approximately 2 g. of 5,8-quinoxalinedione were dissolved in 200 ml. of 2B ethanol. Aniline (1.2 g.) was added and the reaction was stirred overnight at room temperature. The reaction was evaporated, water was added, and the mixture was extracted several times with methylene chloride. The combined extracts were dried over sodium sulfate and evaporated to dryness. The residue was chromatographed over a silica gel column, eluting with ethyl acetate. The desired fractions were combined and evaporated. The material was crystallized from ethyl acetate to give 50 mg. of the title product as a red powder, m.p. about 203°-205° C.

後処理

  1. customThe reaction was evaporated
  2. additionwater was added
  3. extractionthe mixture was extracted several times with methylene chloride
  4. dry with materialThe combined extracts were dried over sodium sulfate
  5. customevaporated to dryness
  6. customThe residue was chromatographed over a silica gel column
  7. washeluting with ethyl acetate
  8. customevaporated
  9. customThe material was crystallized from ethyl acetate
  10. customto give 50 mg

出典と根拠

ORDレコード
ord-fbcec31f3cfc4447831a40bac5b73036
出典データセット
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04486432

反応ノート

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