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

Ethyl Acetate → 2-(2-Fluorophenyl)-3-methyl-N-(2-(4-morpholinyl)-5-(3-thiophenyl)phenyl)-4-quinolinamine

HRID 1431296
ノート
印刷プレビュー

反応式

HRID 1431296 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)=[C:6]([NH:8][C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:12]=[C:11]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[F:25])[C:10]=2[CH3:26])[CH:7]=1.[S:33]1[CH:37]=[CH:36][C:35](B(O)O)=[CH:34]1.C(=O)([O-])[O-].[Na+].[Na+].CCOC(C)=O>O.O1CCOCC1.CCCCCC.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[F:25][C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=1[C:11]1[C:10]([CH3:26])=[C:9]([NH:8][C:6]2[CH:7]=[C:2]([C:35]3[CH:36]=[CH:37][S:33][CH:34]=3)[CH:3]=[CH:4][C:5]=2[N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:12]=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

9

反応物 4

HCID 8857Ethyl AcetateHCID 10340Sodium CarbonateHCID 581760Thiophene-3-boronic acidHCID 59631162N-(5-Bromo-2-morpholinophenyl)-2-(2-fluorophenyl)-3-methylquinolin-4-amine

生成物 1

HCID 509061372-(2-Fluorophenyl)-3-methyl-N-(2-(4-morpholinyl)-5-(3-thiophenyl)phenyl)-4-quinolinamine

試薬・触媒・溶媒 4

HCID 178418476
HCID 178418476、化合物
触媒
HCID 962Water溶媒
HCID 8058Hexane溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
130 °C

実験手順

A mixture of dichlorobis(triphenylphosphine)palladium(II) (13 mg, 18 μmol), N-(5-bromo-2-morpholinophenyl)-2-(2-fluorophenyl)-3-methylquinolin-4-amine (88 mg, 179 μmol), thiophen-3-ylboronic acid (34 mg, 268 μmol) and sodium carbonate (57 mg, 536 μmol) in water (0.25 mL) and 1,4-dioxane (1.00 mL) was purged with nitrogen then heated in a microwave vessel to 130° C. for 60 min, after which time TLC indicated no starting material remained and LC-MS indicated only desired product present. The reaction was partitioned between water and EtOAc (30 mL ea). The organic separation was stirred over anhydrous magnesium sulfate, filtered and the filtrate concentrated under reduced pressure to afford a brown film. The desired product was isolated by chromatography on silica gel eluting isocratically with 33% EtOAc in hexane to afford a colorless solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.99 (2H, dd, J=15.3, 8.2 Hz), 7.79 (1H, s), 7.71 (1H, dd, J=7.0, 7.0 Hz), 7.45-7.63 (5H, m), 7.32-7.45 (2H, m), 7.12-7.29 (3H, m), 6.69 (1H, d, J=1.6 Hz), 3.59 (4H, br. s.), 2.91 (4H, br. s.), 2.06 (3H, d, J=1.6 Hz). Mass Spectrum (ESI) m/e=496.1 (M+1).

後処理

  1. customwas purged with nitrogen
  2. customThe reaction was partitioned between water and EtOAc (30 mL ea)
  3. customThe organic separation
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customto afford a brown film

出典と根拠

ORDレコード
ord-c84a2ad9e7144fe8a957f093a38c2bd1
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08940724B2

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