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Triethylamine → HCID 68909747、化合物

HRID 546545
ノート
印刷プレビュー

反応式

HRID 546545 の反応式
Cl.[CH3:2][O:3][C@H:4]1[C@@H:9]([O:10][CH3:11])[CH2:8][C@@H:7]([NH2:12])[C@@H:6]([NH2:13])[CH2:5]1.Cl.CO[C@@H]1[C@H](OC)C[C@@H](N)[C@@H](N)C1.C(N(CC)CC)C.[Cl:34][C:35]1[CH:36]=[C:37]2[C:41](=[CH:42][CH:43]=1)[NH:40][C:39]([C:44](OC1C=CC([N+]([O-])=O)=CC=1)=[O:45])=[CH:38]2>CN(C)C=O>[Cl:34][C:35]1[CH:36]=[C:37]2[C:41](=[CH:42][CH:43]=1)[NH:40][C:39]([C:44]([NH:12][C@@H:7]1[CH2:8][C@H:9]([O:10][CH3:11])[C@H:4]([O:3][CH3:2])[CH2:5][C@@H:6]1[NH2:13])=[O:45])=[CH:38]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 17842415p-Nitrophenyl 5-chloroindole-2-carboxylateHCID 68907936HCID 68907936、化合物HCID 68909445HCID 68909445、化合物

生成物 1

HCID 68909747HCID 68909747、化合物収率 32.3%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture (645 mg) of (1R*,2S*,4R*,5S*)-4,5-dimethoxy-1,2-cyclohexanediamine hydrochloride and (1R*,2S*,4S*,5R*)-4,5-dimethoxy-1,2-cyclohexane-diamine hydrochloride was suspended in N,N-dimethylformamide (50 ml), and triethylamine (1.10 ml) and p-nitrophenyl 5-chloroindole-2-carboxylate (920 mg) were added to stir the mixture overnight at room temperature. The reaction mixture was concentrated under reduced pressure, and a saturated aqueous solution of sodium hydrogencarbonate was added to the residue to conduct extraction with dichloromethane. The resultant organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (methanol:dichloromethane=1:9) to obtain a mixture (330 mg) of (1R*,2S*,4R*,5S*)-N1-[(5-chloroindol-2-yl)carbonyl]-4,5-dimethoxy-1,2-cyclohexanediamine and (1R*,2S*,4S*,5R*)-N1-[(5-chloroindol-2-yl)carbonyl]-4,5-dimethoxy-1,2-cyclohexanediamine as pale yellow powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additiona saturated aqueous solution of sodium hydrogencarbonate was added to the residue
  3. extractionextraction with dichloromethane
  4. dry with materialThe resultant organic layer was dried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe residue was purified by column chromatography on silica gel (methanol:dichloromethane=1:9)

出典と根拠

ORDレコード
ord-ef102e0be5974e23b51d202eb888270c
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07935824B2

反応ノート

読み込み中…

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