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Sodium Carbonate → HCID 22503541, 화합물

HRID 1251214
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HRID 1251214 반응식
[CH3:1][C:2]1([C:7]2[CH:12]=[CH:11][C:10](OB(O)O)=[CH:9][CH:8]=2)[O:6][CH2:5][CH2:4][O:3]1.Br[C:18]1[N:19]=[C:20]([N:28]2[CH2:33][CH2:32][N:31]([CH2:34][CH3:35])[CH2:30][CH2:29]2)[C:21]2[C:26]([CH:27]=1)=[CH:25][CH:24]=[CH:23][CH:22]=2.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.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>[CH2:34]([N:31]1[CH2:30][CH2:29][N:28]([C:20]2[C:21]3[C:26](=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:27]=[C:18]([C:10]3[CH:11]=[CH:12][C:7]([C:2]4([CH3:1])[O:6][CH2:5][CH2:4][O:3]4)=[CH:8][CH:9]=3)[N:19]=2)[CH2:33][CH2:32]1)[CH3:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 225024471-(1-Ethylpiperazin-4-yl)-3-bromoisoquinolineHCID 22503476HCID 22503476, 화합물

생성물 1

HCID 22503541HCID 22503541, 화합물

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 1140
Toluene
용매

실험 절차

4-(2-Methyl-1,3-dioxolan-2-yl)phenylboric acid (0.41 g) and 3-bromo-1-(4-ethylpiperazin-1-yl)isoquinoline (0.62 g) were reacted in the presence of tetrakistriphenylphosphinepalladium(0) (0.11 g) in toluene (50 ml) and a 10% aqueous solution of sodium carbonate (30 ml) in nitrogen atmosphere at 120° C. for 30 min. The organic layer was separated, washed with brine and dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol system), to give 1-(4-ethylpiperazin-1-yl)-3-[4-(2-methyl-l,3-dioxolan-2-yl)phenyl]isoquinoline.

후처리

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated
  5. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol system)

출처 및 근거

ORD 기록
ord-4defb41da99b4cd696e7bad18275717a
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06340759B1

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