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Ethanol → 2-(2-(2,3-Dihydrobenzofuran-5-yl)ethyl)-8-methylbenzo[f][1,7]naphthyridin-5-amine

HRID 1259124
ノート
印刷プレビュー

反応式

HRID 1259124 の反応式
N1[C:9]2[C:4](=[CH:5][C:6]([C:10]#[C:11][C:12]3[CH:13]=[N:14][C:15]4[C:20]([CH:21]=3)=[C:19]3[CH:22]=[CH:23][C:24]([CH3:26])=[CH:25][C:18]3=[N:17][C:16]=4[NH2:27])=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.C([OH:30])C.[H][H]>[Pd].C(Cl)Cl>[O:30]1[C:9]2[CH:8]=[CH:7][C:6]([CH2:10][CH2:11][C:12]3[CH:13]=[N:14][C:15]4[C:20]([CH:21]=3)=[C:19]3[CH:22]=[CH:23][C:24]([CH3:26])=[CH:25][C:18]3=[N:17][C:16]=4[NH2:27])=[CH:5][C:4]=2[CH2:3][CH2:2]1
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 3

HCID 702EthanolHCID 668930492-((1H-indol-5-yl)ethynyl)-8-methylbenzo[f][1,7]naphthyridin-5-amineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 442314112-(2-(2,3-Dihydrobenzofuran-5-yl)ethyl)-8-methylbenzo[f][1,7]naphthyridin-5-amine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 6344
Dichloromethane
溶媒

実験手順

To a round bottom flask was added 2-((1H-indol-5-yl)ethynyl)-8-methylbenzo[f][1,7]naphthyridin-5-amine (from the previous step) (1 eq.) with a stirring bar. Ethanol and methylene chloride (1:2, 0.2 M) were added, followed by palladium in carbon (activated powder, wet, 10% on carbon, 0.1 eq.). The content were vacuumed followed by hydrogen flush for three times. The reaction mixture was stirred vigorously under hydrogen balloon at room temperature overnight. Afterwards the reaction mixture was filtered through a celite pad, and the celite pad was washed subsequently with methylene chloride and EtOAc until the filtrate had no UV absorption. Combined organic washes were concentrated. Flash chromatography (silica gel, 0-50% EtOAc in CH2Cl2) afforded the product 2-(2-(2,3-Dihydrobenzofuran-5-yl)ethyl)-8-methylbenzo[f][1,7]naphthyridin-5-amine as a yellow solid. 1H NMR (CDCl3): δ 8.54 (d, 1H), 8.34 (d, 1H), 8.28 (s, 1H), 7.99 (d, 1H), 7.64-7.56 (m, 1H), 7.50-7.35 (m, 1H), 7.24 (d, 1H), 7.12 (t, 1H), 7.08 (dd, 1H), 6.92 (dd, 1H), 6.41 (s, 1H), 6.01 (bs, 2H), 3.16-3.12 (m, 2H), 3.10-3.05 (m, 2H), 2.43 (s, 3H). LRMS [M+H]=353.2

後処理

  1. customflush for three times
  2. filtrationAfterwards the reaction mixture was filtered through a celite pad
  3. washthe celite pad was washed subsequently with methylene chloride and EtOAc until the filtrate
  4. customno UV absorption
  5. concentrationCombined organic washes were concentrated

出典と根拠

ORDレコード
ord-bb69f8c363f5438fa3804f85f9cc695a
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08466167B2

反応ノート

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