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Aniline → HCID 9816404, 화합물

HRID 1153731
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HRID 1153731 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6115AnilineHCID 113556455,8-Quinoxalinedione

생성물 1

HCID 9816404HCID 9816404, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fbcec31f3cfc4447831a40bac5b73036
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04486432

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