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

Dimethylformamide → Diethyl 2-(2',3-dimethyl-2,4'-bipyridin-5-yl)malonate

HRID 592184
ノート
印刷プレビュー

反応式

HRID 592184 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([CH:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:4][C:3]=1[CH3:19].[CH3:20][C:21]1[CH:26]=[C:25]([Sn](CCCC)(CCCC)CCCC)[CH:24]=[CH:23][N:22]=1.CN(C=O)C.[F-].[K+]>C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:20][C:21]1[CH:26]=[C:25]([C:2]2[C:3]([CH3:19])=[CH:4][C:5]([CH:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:6][N:7]=2)[CH:24]=[CH:23][N:22]=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

7

反応物 4

HCID 6228DimethylformamideHCID 522689Potassium FluorideHCID 216605742-Methyl-4-(tributylstannyl)pyridineHCID 58447937Diethyl 2-(6-chloro-5-methylpyridin-3-yl)malonate

生成物 1

HCID 58447640Diethyl 2-(2',3-dimethyl-2,4'-bipyridin-5-yl)malonate

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

To a reaction flask containing diethyl 2-(6-chloro-5-methylpyridin-3-yl)malonate 156-3 (1.00 g, 4.00 mmol), 2-methyl-4-(tributylstannyl)pyridine (1.53 g, 4.00 mmol) and Pd(PPh3)4 (440 mg, 0.4 mmol) under argon was added DMF (20 mL). The mixture was stirred at 120° C. for 10 hours. After the mixture was cooled down to room temperature, 1N KF aqueous solution was added to it and stirred for 15 minutes. The mixture was diluted with ethyl acetate and the two layers were separated. The organic layer was further washed with water and brine, dried over Na2SO4, concentrated to dryness by rotary evaporation. The crude product was purified by silica gel flash chromatography, eluted with 5% methanol in dichloromethane to give diethyl 2-(2′,3-dimethyl-2,4′-bipyridin-5-yl)malonate 156-4 as colorless oil. MS m/z 343.1 (M+1)

後処理

  1. temperatureAfter the mixture was cooled down to room temperature
  2. stirringstirred for 15 minutes
  3. customthe two layers were separated
  4. washThe organic layer was further washed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated to dryness by rotary evaporation
  7. customThe crude product was purified by silica gel flash chromatography
  8. washeluted with 5% methanol in dichloromethane

出典と根拠

ORDレコード
ord-691b6da43a8b481bb483f63b36ecb242
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09238646B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート