Water → HCID 16666575, 화합물

HRID 1511819

반응식

HRID 1511819 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 16666575HCID 16666575, 화합물

시약·촉매·용매 2

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

반응 조건

온도
90 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-bb836e82f9204d52b9a74b7116952c80
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217042B2

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