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 → HCID 86690474、化合物

HRID 1026749
ノート
印刷プレビュー

反応式

HRID 1026749 の反応式
Br[C:2]1[CH:7]=[C:6]([CH2:8][NH:9][CH:10]([CH3:12])[CH3:11])[CH:5]=[CH:4][N:3]=1.[F:13][C:14]1[CH:19]=[CH:18][C:17](B(O)O)=[CH:16][CH:15]=1.C(=O)([O-])[O-].[Cs+].[Cs+].C(=O)([O-])O.[Na+]>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.C(OCC)(=O)C.O.C(O)C.C1(C)C=CC=CC=1>[F:13][C:14]1[CH:19]=[CH:18][C:17]([C:2]2[CH:7]=[C:6]([CH2:8][NH:9][CH:10]([CH3:12])[CH3:11])[CH:5]=[CH:4][N:3]=2)=[CH:16][CH:15]=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

10

反応物 4

HCID 10796Cesium carbonateHCID 2856454-Fluorophenylboronic acidHCID 516892Sodium BicarbonateHCID 53385538N-[(2-Bromopyridin-4-yl)methyl]propan-2-amine

生成物 1

HCID 86690474HCID 86690474、化合物収率 53%

試薬・触媒・溶媒 5

HCID 178418397
HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
150 °C

実験手順

A mixture of N-[(2-bromopyridin-4-yl)methyl]propan-2-amine (2.00 g), 4-fluorophenylboronic acid (1.34 g), cesium carbonate (4.26 g), tetrakis(triphenylphosphine)palladium (1.01 g), toluene (4.5 mL), ethanol (4.5 mL) and water (3.0 mL) was stirred under irradiation with microwave while heating at 150° C. for 30 min. Saturated aqueous sodium hydrogen carbonate solution and ethyl acetate were added to the reaction mixture, and the resulting mixture was then filtered through Celite and extracted with ethyl acetate. The whole organic phase was collected and dried over magnesium sulfate. After the desiccant was filtered off, the solution was concentrated under reduced pressure. The resulting residue was purified by column chromatography (silica gel cartridge, chloroform:methanol=96:4-92:8) and (NH silica gel cartridge, hexane:ethyl acetate=90:10-60:40) to afford the title compound (1.13 g).

後処理

  1. filtrationthe resulting mixture was then filtered through Celite
  2. extractionextracted with ethyl acetate
  3. customThe whole organic phase was collected
  4. dry with materialdried over magnesium sulfate
  5. filtrationAfter the desiccant was filtered off
  6. concentrationthe solution was concentrated under reduced pressure
  7. customThe resulting residue was purified by column chromatography (silica gel cartridge, chloroform:methanol=96:4-92:8) and (NH silica gel cartridge, hexane:ethyl acetate=90:10-60:40)

出典と根拠

ORDレコード
ord-e92c977e3fae4cef8c68e551f184cff5
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08729271B2

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