ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Methyl iodide → 1-(4-(6,7-Dimethoxyquinolin-4-yloxy)-3-fluorophenyl)-4-(methoxy(phenyl)methyl)pyrrolidin-2-one

HRID 1993389
ノート
印刷プレビュー

反応式

HRID 1993389 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]2[CH2:26][CH:25]([CH:27]([OH:34])[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[CH2:24][C:23]2=[O:35])=[CH:18][C:17]=1[F:36].[H-].[Na+].[CH3:39]I>C1COCC1.CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]2[CH2:26][CH:25]([CH:27]([O:34][CH3:39])[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[CH2:24][C:23]2=[O:35])=[CH:18][C:17]=1[F:36]
参加物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 6328Methyl iodideHCID 24758Sodium hydrideHCID 587517811-(4-(6,7-Dimethoxyquinolin-4-yloxy)-3-fluorophenyl)-4-(hydroxy(phenyl)methyl)pyrrolidin-2-one

生成物 1

HCID 118577281-(4-(6,7-Dimethoxyquinolin-4-yloxy)-3-fluorophenyl)-4-(methoxy(phenyl)methyl)pyrrolidin-2-one

試薬・触媒・溶媒 1

HCID 21974620tetrahydrofuran N,N-dimethylformamide
溶媒

実験手順

To a solution of 1-(4-(6,7-dimethoxyquinolin-4-yloxy)-3-fluorophenyl)-4-(hydroxy(phenyl)methyl)pyrrolidin-2-one (Example 48, 0.1 g, 0.2 mmol) in THF/DMF (1 mL:1 mL) was added NaH (0.1 g, 2.5 mmol) solid. The reaction was stirred at RT for 1 h. MeI (0.1 mL, 1.6 mmol) was added via a syringe and the reaction was stirred for 1 h. The reaction was quenched with 10 mL of satd. NH4Cl solution and 10 mL of water. The solution was diluted with 50 mL of EtOAc. The organic phase was separated and was washed with 30 mL of brine, dried over Na2SO4 and concentrated in vacuo. The crude oil was purified by chromatography (10% EtOAc/hexanes to EtOAc) to give colorless film. MS (ESI pos. ion) m/z: 503.5 (M+H). Calc'd Exact Mass for C29H27FN2O5: 502.53.

後処理

  1. stirringthe reaction was stirred for 1 h
  2. customThe reaction was quenched with 10 mL of satd
  3. additionThe solution was diluted with 50 mL of EtOAc
  4. customThe organic phase was separated
  5. washwas washed with 30 mL of brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo
  8. customThe crude oil was purified by chromatography (10% EtOAc/hexanes to EtOAc)
  9. customto give colorless film

出典と根拠

ORDレコード
ord-b56710e1e17a45a6b032a227839e4c85
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07652009B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート