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

Water → N-(2-(2-chlorophenyl)-4-oxo-1,4-dihydro-1,7-naphthyridin-6-yl)cyclopropanecarboxamide

HRID 468846
ノート
印刷プレビュー

反応式

HRID 468846 の反応式
Cl[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][N:11]=1)[NH:8][C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:18])=[CH:6][C:5]2=[O:19].[CH:20]1([C:23]([NH2:25])=[O:24])[CH2:22][CH2:21]1.C(=O)([O-])[O-].[Cs+].[Cs+].O>O1CCOCC1.[Cl-].[Na+].O>[Cl:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[C:7]1[NH:8][C:9]2[C:4]([C:5](=[O:19])[CH:6]=1)=[CH:3][C:2]([NH:25][C:23]([CH:20]1[CH2:22][CH2:21]1)=[O:24])=[N:11][CH:10]=2
参加物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 962WaterHCID 10796Cesium carbonateHCID 80376Cyclopropanecarboxamide2 回HCID 866749476-chloro-2-(2-chlorophenyl)-1,7-naphthyridin-4(1H)-one

生成物 1

HCID 67977259N-(2-(2-chlorophenyl)-4-oxo-1,4-dihydro-1,7-naphthyridin-6-yl)cyclopropanecarboxamide収率 6.2%

試薬・触媒・溶媒 2

HCID 31275
1,4-Dioxane
溶媒
HCID 57417360Sodium chloride; water溶媒

実験手順

A mixture of 6-chloro-2-(2-chlorophenyl)-1,7-naphthyridin-4(1H)-one (29.2 mg, 100 μmol), cyclopropanecarboxamide (17.1 mg, 200 μmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl][2-(2-aminoeth yl)phenyl]palladium(II) (8.0 mg, 10 μmol), 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl (5.4 mg, 10 μmol), and cesium carbonate (98.0 mg, 301 μmol) in 1,4-dioxane (5.0 mL) was heated to reflux for 4 hours. Further portions of cyclopropanecarboxamide (17.1 mg, 200 μmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl][2-(2-aminoeth yl)phenyl]palladium(II) (8.0 mg, 10 μmol) and 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl (5.4 mg, 10 μmol) were added and the mixture heated to reflux for 16 hours. The cooled mixture was treated with water and brine and extracted with ethyl acetate, and the separated organic phase washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by reverse phase HPLC (gradient of acetonitrile in water with 0.1% formic acid) to afford the title compound as a white solid (2.1 mg, 6.2%). LCMS (Method E): RT=3.715 min, M+H+=340.0 & 342.0.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 4 hours
  3. temperaturethe mixture heated
  4. temperatureto reflux for 16 hours
  5. extractionextracted with ethyl acetate
  6. washthe separated organic phase washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified by reverse phase HPLC (gradient of acetonitrile in water with 0.1% formic acid)

出典と根拠

ORDレコード
ord-ec2c039f7a5f43f89bb96ebc222bfb74
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08623889B2

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