Water → HCID 16666575、化合物

HRID 1511819ノート

反応式

HRID 1511819 の反応式
Cl[C:2]1[N:7]=[C:6]2[N:8]=[C:9]([NH:12][C:13]([NH:15][CH2:16][CH3:17])=[O:14])[CH:10]=[CH:11][C:5]2=[N:4][CH:3]=1.[CH:18]1([CH:24]=[CH:25]B(O)O)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[Na+].[Na+].O>CN(C)C=O.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH:18]1(/[CH:24]=[CH:25]/[C:2]2[N:7]=[C:6]3[N:8]=[C:9]([NH:12][C:13]([NH:15][CH2:16][CH3:17])=[O:14])[CH:10]=[CH:11][C:5]3=[N:4][CH:3]=2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1

参加物

7

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 41851492-Cyclohexylvinyl boronic acidHCID 588817911-(3-Chloropyrido[2,3-b]pyrazin-6-yl)-3-ethylurea

生成物 1

HCID 16666575HCID 16666575、化合物

試薬・触媒・溶媒 2

HCID 178418228Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 21962138N,N-Dimethylformamide--water (1/1)溶媒

反応条件

温度
90 °C

実験手順

99.6 mg of 1-(3-chloropyrido[2,3-b]pyrazin-6-yl)-3-ethylurea (0.40 mmol), 73.6 mg of cyclohexylvinylboronic acid (0.48 mmol), 84.4 mg of sodium carbonate (0.80 mmol) and 33.4 mg of [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (0.04 mmol) were initially charged in 6 ml of dimethylformamide/water (1:1) under nitrogen. The mixture was then heated to 90° C. for 6.5 h. Distilled water was then added to the reaction mixture and the resulting precipitate was filtered off with suction. The further purification was effected by column chromatography on silica gel (ethyl acetate/heptane eluent mixture). A light brown solid was obtained.

後処理

  1. filtrationthe resulting precipitate was filtered off with suction
  2. customThe further purification
  3. customA light brown solid was obtained

出典と根拠

ORDレコード
ord-bb836e82f9204d52b9a74b7116952c80
出典データセット
uspto-grants-2012_07
特許番号
US08217042B2

反応ノート

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