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Diisopropylethylamine → trans-2-(4-Chloro-benzenesulfonylamino)-cyclohexanecarboxylic acid [cyano-(3-hydroxy-phenyl)-methyl]-amide

HRID 990914
ノート
印刷プレビュー

反応式

HRID 990914 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C@@H:12]2[CH2:17][CH2:16][CH2:15][CH2:14][C@H:13]2[C:18]([OH:20])=O)(=[O:10])=[O:9])=[CH:4][CH:3]=1.F[B-](F)(F)F.C[N+](C)=C(N(C)C)O.C(N(C(C)C)C(C)C)C.[NH2:43][CH:44]([C:47]1[CH:52]=[CH:51][CH:50]=[C:49]([OH:53])[CH:48]=1)[C:45]#[N:46]>CC#N>[C:45]([CH:44]([NH:43][C:18]([C@@H:13]1[CH2:14][CH2:15][CH2:16][CH2:17][C@H:12]1[NH:11][S:8]([C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1)(=[O:9])=[O:10])=[O:20])[C:47]1[CH:52]=[CH:51][CH:50]=[C:49]([OH:53])[CH:48]=1)#[N:46]
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 81531DiisopropylethylamineHCID 13074157Tetramethyluronium tetrafluoroborateHCID 16793683Amino-(3-hydroxy-phenyl)-acetonitrileHCID 69656371Trans-2-(4-Chloro-benzenesulfonylamino)-cyclohexanecarboxylic acid

生成物 1

HCID 10182237trans-2-(4-Chloro-benzenesulfonylamino)-cyclohexanecarboxylic acid [cyano-(3-hydroxy-phenyl)-methyl]-amide

試薬・触媒・溶媒

1
HCID 6342Acetonitrile溶媒2 回

実験手順

Trans-2-(4-Chloro-benzenesulfonylamino)-cyclohexanecarboxylic acid (0.095 g, 0.3 mmol) is dissolved in CH3CN. O-1,2-Dihydro-2-oxo-1-pyridyl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (TPTU, 90.2 mg, 0.3 mmol), N-Ethyldiisopropylamine (DIPEA, 0.208 ml, 1.21 mmol) are added. The amino-(3-hydroxy-phenyl)-acetonitrile in CH3CN (1.5 ml) is added. The mixture is stirred at RT for 16 hours. The solution is filtered and concentrated. The residue is dissolved in CH2Cl2 (15 mL) and extracted with NH4Cl (2×10 ml). The H2O layers are extracted with CH2Cl2 (2×15 ml). The collected CH2Cl2 layers are dried over MgSO4 and evaporated. The solid is purified by preparative HPLC.

後処理

  1. filtrationThe solution is filtered
  2. concentrationconcentrated
  3. dissolutionThe residue is dissolved in CH2Cl2 (15 mL)
  4. extractionextracted with NH4Cl (2×10 ml)
  5. extractionThe H2O layers are extracted with CH2Cl2 (2×15 ml)
  6. dry with materialThe collected CH2Cl2 layers are dried over MgSO4
  7. customevaporated
  8. customThe solid is purified by preparative HPLC

出典と根拠

ORDレコード
ord-caf89cdf3d194145a88fa364620632ac
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06462076B2

反応ノート

読み込み中…

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