N-Methylcyclohexylamine → N-Cyclohexyl-3, N-dimethyl-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate salt

HRID 2268625ノート

反応式

HRID 2268625 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH3:8][C:9]1[CH:10]=[C:11]([CH:15]=[C:16]([O:18][CH2:19][CH2:20][NH:21][C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)[CH:17]=1)[C:12]([OH:14])=O.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C.[CH3:47][NH:48][CH:49]1[CH2:54][CH2:53][CH2:52][CH2:51][CH2:50]1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F>CN(C=O)C>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH:49]1([N:48]([CH3:47])[C:12](=[O:14])[C:11]2[CH:15]=[C:16]([O:18][CH2:19][CH2:20][NH:21][C:22]3[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=3)[CH:17]=[C:9]([CH3:8])[CH:10]=2)[CH2:54][CH2:53][CH2:52][CH2:51][CH2:50]1

参加物

7

反応物 5

HCID 7514N-MethylcyclohexylamineHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 699496943-Methyl-5-[2-(pyridin-4-ylamino)-ethoxy]-benzoic acid trifluoroacetate

生成物 1

HCID 17899506N-Cyclohexyl-3, N-dimethyl-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate salt

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A stirred solution of 3-methyl-5-[2-(pyridin-4-ylamino)-ethoxy]-benzoic acid trifluoroacetate salt (0.031 g) in DMF (1 ml) was treated with HOBt (0.011 g), DIPEA (0.028 ml), N-methylcyclohexylamine (0.010 ml), and TBTU (0.026 g). The resulting solution was retained in a sealed flask for 64 h. The reaction mixture was concentrated under reduced pressure and the resulting gum subjected to preparative hplc. The required fraction was concentrated and then dried by addition of methanol and concentration under reduced pressure, addition of toluene and again concentration under reduced pressure giving the title compound as a colourless gum (0.034 g).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. concentrationThe required fraction was concentrated
  3. dry with materialdried by addition of methanol and concentration under reduced pressure, addition of toluene and again concentration under reduced pressure

出典と根拠

ORDレコード
ord-b8f9bcffdf264b1b9615023c17e7936a
出典データセット
uspto-grants-2001_12
特許番号
US06326386B1

反応ノート

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