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Sodium hydride → 2-(3-(Pyridin-3-yl)benzyl)-9-(quinoxalin-2-yl)-2,9-diazaspiro[5.5]undecan-1-one

HRID 41545
ノート
印刷プレビュー

反応式

HRID 41545 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]=[CH:3][C:2]=1[N:11]1[CH2:22][CH2:21][C:14]2([C:19](=[O:20])[NH:18][CH2:17][CH2:16][CH2:15]2)[CH2:13][CH2:12]1.[H-].[Na+].Cl[CH2:26][C:27]1[CH:28]=[C:29]([C:33]2[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=2)[CH:30]=[CH:31][CH:32]=1>C1COCC1>[N:35]1[CH:36]=[CH:37][CH:38]=[C:33]([C:29]2[CH:28]=[C:27]([CH:32]=[CH:31][CH:30]=2)[CH2:26][N:18]2[CH2:17][CH2:16][CH2:15][C:14]3([CH2:21][CH2:22][N:11]([C:2]4[CH:3]=[N:4][C:5]5[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=5)[N:1]=4)[CH2:12][CH2:13]3)[C:19]2=[O:20])[CH:34]=1
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

5

反応物 3

HCID 24758Sodium hydrideHCID 190793993-(3-Chloromethyl-phenyl)-pyridineHCID 672517459-(Quinoxalin-2-yl)-2,9-diazaspiro[5.5]undecan-1-one

生成物 1

HCID 532592782-(3-(Pyridin-3-yl)benzyl)-9-(quinoxalin-2-yl)-2,9-diazaspiro[5.5]undecan-1-one収率 46%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

To a stirred solution of 9-(quinoxalin-2-yl)-2,9-diazaspiro[5.5]undecan-1-one (0.035 g, 0.12 mmol) in dry THF (4.0 mL), NaH (0.014 g, 0.36 mmol) was added at rt and the mixture was stirred for 10 min. 3-(3-Chloromethyl-phenyl)-pyridine (0.05 g, 0.24 mmol) was then added and the reaction mixture was heated to 60° C. for 6 h. The mixture was quenched with 1 ml saturated aqueous NH4Cl solution, diluted with 50 ml water and the resulting mixture was extracted with ethyl acetate (100 mL). The organic layer was washed with water and brine. The organic layer was dried over Na2SO4, filtered and concentrated to obtain the crude product. Preparative HPLC purification furnished the title compound as a pale yellow sticky solid (0.025 g, 46%). [1H-NMR (CDCl3, 300 MHz): δ 8.84-8.81 (m, 1H), 8.66-8.58 (m, 2H), 7.92-7.81 (m, 2H), 7.72-7.65 (m, 1H), 7.35-7.61 (m, 6H), 4.68 (s, 2H), 4.31-4.20 (m, 2H), 3.70-3.55 (m, 2H), 3.31 (t, 2H), 2.43-2.29 (m, 2H), 1.96-1.82 (m, 4H), 1.75-1.63 (dt, 2H); HPLC RtA=4.635 min (96%); LCMS RtC=0.395, [M+H]+=464.0].

後処理

  1. customThe mixture was quenched with 1 ml saturated aqueous NH4Cl solution
  2. additiondiluted with 50 ml water
  3. extractionthe resulting mixture was extracted with ethyl acetate (100 mL)
  4. washThe organic layer was washed with water and brine
  5. dry with materialThe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto obtain the crude product
  9. customPreparative HPLC purification

出典と根拠

ORDレコード
ord-83a33ac8b4e64bb0b31f91bf4324c79f
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08530648B2

反応ノート

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