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Ammonia → HCID 25184712、化合物

HRID 1878066
ノート
印刷プレビュー

反応式

HRID 1878066 の反応式
[Cl:1][CH2:2][C:3]([NH:5][C:6]1[CH:7]=[N:8][C:9]([C:12](=[N:14][OH:15])[NH2:13])=[CH:10][CH:11]=1)=[O:4].N.[C:17](OC(=O)C)(=O)[CH3:18]>O>[Cl:1][CH2:2][C:3]([NH:5][C:6]1[CH:7]=[N:8][C:9]([C:12]2[N:13]=[C:17]([CH3:18])[O:15][N:14]=2)=[CH:10][CH:11]=1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 222AmmoniaHCID 7918Acetic AnhydrideHCID 137068883HCID 137068883、化合物

生成物 1

HCID 25184712HCID 25184712、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Compound of example 4 (5.5 g, 24 mmol) was refluxed in acetic anhydride (10 mL) at a temperature in the range of 115-120° C. for 2 hours. The black colored reaction mixture was cooled, diluted with water, basified with ammonia solution, and extracted with ethyl acetate (3×100 mL). The organic layer was washed with brine, dried over sodium sulfate and concentrated. The crude product obtained was purified over silica gel using ethyl acetate/petroleum ether (25%-50%) as eluent and the semipurified fractions were further purified using methanol/chloroform (0.5% -1%) as eluent. Pure fractions were concentrated and crystallized using chloroform/petroleum ether, to obtain the title compound.

後処理

  1. temperatureThe black colored reaction mixture was cooled
  2. extractionextracted with ethyl acetate (3×100 mL)
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe crude product obtained
  7. customwas purified over silica gel
  8. customthe semipurified fractions were further purified
  9. concentrationPure fractions were concentrated
  10. customcrystallized

出典と根拠

ORDレコード
ord-724c10d5fe54499e984e8ef8c4090265
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08314103B2

反応ノート

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