Tetrahydrofuran → HCID 178526691、化合物

HRID 22941

反応式

HRID 22941 の反応式
O1CCCC1.[NH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([OH:13])[CH2:9][CH2:8]1.C(N(CC)CC)C.Cl[C:22]1[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][N:23]=1>O>[N+:28]([C:25]1[CH:26]=[CH:27][C:22]([NH:6][C@H:7]2[CH2:12][CH2:11][C@H:10]([OH:13])[CH2:9][CH2:8]2)=[N:23][CH:24]=1)([O-:30])=[O:29]

参加物

6

反応物 4

HCID 8028Tetrahydrofuran2 回HCID 8471TriethylamineHCID 783082-Chloro-5-nitropyridineHCID 178511715HCID 178511715、化合物

生成物 1

HCID 178526691HCID 178526691、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 150 ml of a tetrahydrofuran suspension containing 10 g of trans-4-aminocyclohexanol was added 15ml of triethylamine, 50 ml of a tetrahydrofuran solution containing 2-chloro-5-nitropyridine was further added thereto under ice-cooling, and then, the mixture was stirred at room temperature for 18 hours. Water was added to the reaction mixture and the mixture was extracted with chloroform. The extract was washed with brine, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The residue was purified by silica gel flash column chromatography (solvent: ethyl acetate-hexane (2:1)) to obtain 8.52 g of trans-4-(5-nitro-2-pyridylamino)cyclohexanol.

後処理

  1. additionwas further added
  2. temperatureunder ice-cooling
  3. extractionthe mixture was extracted with chloroform
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by silica gel flash column chromatography (solvent: ethyl acetate-hexane (2:1))

出典と根拠

ORDレコード
ord-bacd710fc5fe481bbf029ea3a08e93f4
出典データセット
uspto-grants-2005_02
特許番号
US06849622B2

関連ノート

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