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N-Methylcyclohexylamine → 5-Cyano-6-(2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid cyclohexyl-methyl-amide

HRID 502865
ノート
印刷プレビュー

反応式

HRID 502865 の反応式
[C:1]([C:3](=[CH:16][C:17]1[CH:22]=[C:21]([O:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:20]=[CH:19][C:18]=1[N+:30]([O-:32])=[O:31])[CH:4]([CH:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1)[CH2:5][CH2:6][C:7]([OH:9])=O)#[N:2].[CH3:33][NH:34][CH:35]1[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C>[CH:35]1([N:34]([CH3:33])[C:7](=[O:9])[CH2:6][CH2:5][CH:4]([CH:10]2[CH2:11][CH2:12][O:13][CH2:14][CH2:15]2)[C:3]([C:1]#[N:2])=[CH:16][C:17]2[CH:22]=[C:21]([O:23][C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH:20]=[CH:19][C:18]=2[N+:30]([O-:32])=[O:31])[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7514N-MethylcyclohexylamineHCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 672694525-Cyano-6-(2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid

生成物 1

HCID 67269340
5-Cyano-6-(2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid cyclohexyl-methyl-amide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 5-cyano-6-(2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid (0.87 g, 2 mmol), N-methylcyclohexylamine (0.26 mL, 2 mmol), HBTU (1.13 g, 3 mmol), DIPEA (1.2 mL, 7 mmol) in DMF (20 mL) was stirred at room temperature overnight. Ethyl acetate was added to the reaction mixture. The solution washed with saturated aqueous NaHCO3 solution. The organic phase was separated and dried with MgSO4, and filtered. The solvent was removed in vacuo to yield the title compound as an oil.

後処理

  1. washThe solution washed with saturated aqueous NaHCO3 solution
  2. customThe organic phase was separated
  3. dry with materialdried with MgSO4
  4. filtrationfiltered
  5. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-4c3d833126d444168f6bce87a78dc29d
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776882B2

反応ノート

読み込み中…

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