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

Cesium carbonate → 1-(4-Chloro-5,7-difluoro-3-methylquinolin-2-yl)-5,5-dimethylpiperidin-2-one

HRID 1618749
ノート
印刷プレビュー

反応式

HRID 1618749 の反応式
CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.Cl[C:44]1[C:53]([CH3:54])=[C:52]([Cl:55])[C:51]2[C:46](=[CH:47][C:48]([F:57])=[CH:49][C:50]=2[F:56])[N:45]=1.[CH3:58][C:59]1([CH3:66])[CH2:64][NH:63][C:62](=[O:65])[CH2:61][CH2:60]1.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.CCOC(C)=O.C(Cl)Cl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:55][C:52]1[C:51]2[C:46](=[CH:47][C:48]([F:57])=[CH:49][C:50]=2[F:56])[N:45]=[C:44]([N:63]2[CH2:64][C:59]([CH3:66])([CH3:58])[CH2:60][CH2:61][C:62]2=[O:65])[C:53]=1[CH3:54]
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 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 104796605,5-Dimethylpiperidin-2-oneHCID 596310402,4-Dichloro-5,7-difluoro-3-methylquinoline

生成物 1

HCID 596312031-(4-Chloro-5,7-difluoro-3-methylquinolin-2-yl)-5,5-dimethylpiperidin-2-one

試薬・触媒・溶媒 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 6344Dichloromethane溶媒
HCID 8857Ethyl Acetate溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

XantPhos (273 mg, 0.472 mmol), 2,4-dichloro-5,7-difluoro-3-methylquinoline (780 mg, 3.20 mmol), 5,5-dimethylpiperidin-2-one (400 mg, 3.20 mmol), cesium carbonate (1.40 g, 4.40 mmol) and Pd2(dba)3 (140 mg, 0.160 mmol) was slurried in 1,4-dioxane (8.5 mL) and heated in a microwave reactor at 100° C. for 3 h. The reaction was cooled to rt and then diluted with EtOAc and DCM. The slurry was then filtered and concentrated. The residue was purified by column chromatography (silica gel, 0 to 50% EtOAc:DCM) to give 1-(4-chloro-5,7-difluoro-3-methylquinolin-2-yl)-5,5-dimethylpiperidin-2-one. Mass Spectrum (ESI) m/e=339.1 (M+1).

後処理

  1. temperatureThe reaction was cooled to rt
  2. filtrationThe slurry was then filtered
  3. concentrationconcentrated
  4. customThe residue was purified by column chromatography (silica gel, 0 to 50% EtOAc:DCM)

出典と根拠

ORDレコード
ord-3af9e594ae674cc684d1e47bef10ed7a
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765940B2

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