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Ethanolamine → 2-Amino-6-(4-chloro-benzylamino)-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide

HRID 2080196
ノート
印刷プレビュー

反応式

HRID 2080196 の反応式
[NH2:1][C:2]1[N:23]=[C:22](Cl)[CH:21]=[CH:20][C:3]=1[C:4]([NH:6][CH2:7][C:8]1[S:9][C:10]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:11][CH:12]=1)=[O:5].C1C=CC(CC(NCN[C@H](C(O)=O)CC2C=CC([N+]([O-])=O)=CC=2)=O)=CC=1.[Cl:51][C:52]1[CH:59]=[CH:58][C:55]([CH2:56][NH2:57])=[CH:54][CH:53]=1.C(N(CC)C(C)C)(C)C.C(CN)O.FC(F)(F)C(O)=O>CS(C)=O.O>[NH2:1][C:2]1[N:23]=[C:22]([NH:57][CH2:56][C:55]2[CH:58]=[CH:59][C:52]([Cl:51])=[CH:53][CH:54]=2)[CH:21]=[CH:20][C:3]=1[C:4]([NH:6][CH2:7][C:8]1[S:9][C:10]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:11][CH:12]=1)=[O:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 700EthanolamineHCID 6422Trifluoroacetic acidHCID 660364-ChlorobenzylamineHCID 81531Diisopropylethylamine2 回HCID 188218A-101HCID 231304982-aminochloro-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide

生成物 1

HCID 23130810
2-Amino-6-(4-chloro-benzylamino)-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide
収率 24%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

To a solution of 2-amino-6-chloro-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide described in Example A-101 (35 mg, 0.10 mmol) in dimethylsulfoxide (1mL) were added 4-chlorobenzylamine (234 μl, 1.92 mmol) and N,N-diisopropylethylamine (1.0 mL, 5.74 mmol), and the solution was stirred at 140° C. for 2.5 days. Ethanolamine (116 μl, 1.92 mmol) and N,N-diisopropylethylamine (1.0 mL, 5.74 mmol) were added to the reaction mixture, which was then further stirred at 140° C. for 2.5 days. Water was added to the reaction mixture, which was then extracted with ethyl acetate, the organic layer was sequentially washed with water and brine, dried over anhydrous sodium sulfate, and then, concentrated in vacuo. The obtained residue was purified by reverse phase high performance liquid chromatography (acetonitrile-water mobile phase (containing 0.1% trifluoroacetic acid) was used), and the title compound (13.8 mg, 0.024 mmol, 24%) was obtained as a trifluoroacetic acid salt.

後処理

  1. stirringwas then further stirred at 140° C. for 2.5 days
  2. extractionwas then extracted with ethyl acetate
  3. washthe organic layer was sequentially washed with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe obtained residue was purified by reverse phase high performance liquid chromatography (acetonitrile-water mobile phase (containing 0.1% trifluoroacetic acid) was used)

出典と根拠

ORDレコード
ord-d88497f801ef4f488061673c3d0b26d8
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932272B2

反応ノート

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