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Potassium Carbonate → HCID 136597126, 화합물

HRID 2205197
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HRID 2205197 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([C:11]3[N:12](S(C4C=CC(C)=CC=4)(=O)=O)[C:13]4[C:18]([CH:19]=3)=[CH:17][C:16]([O:20][CH3:21])=[C:15]([O:22][CH3:23])[CH:14]=4)=[CH:9][N:10]=2)[N:7]=1.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.[C:76](=[O:79])([O-])[O-].[K+].[K+].CO[C:84]1[CH:85]=[C:86]([CH:88]=[CH:89][C:90]=1[O:91][CH3:92])[NH2:87]>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:21][O:20][C:16]1[CH:17]=[C:18]2[C:13](=[CH:14][C:15]=1[O:22][CH3:23])[NH:12][C:11]([C:8]1[N:6]3[N:7]=[C:2]([NH:87][C:86]4[CH:88]=[CH:89][C:90]([O:91][CH3:92])=[C:84]([O:79][CH3:76])[CH:85]=4)[CH:3]=[CH:4][C:5]3=[N:10][CH:9]=1)=[CH:19]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 227703,4-DimethoxyanilineHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 90388062HCID 90388062, 화합물

생성물 1

HCID 136597126HCID 136597126, 화합물수율 31.8%

시약·촉매·용매 2

HCID 167845
palladium(II) acetate
촉매
HCID 312751,4-Dioxane용매

반응 조건

온도
110 °C

실험 절차

To a solution of 6-chloro-3-(5,6-dimethoxy-1-tosyl-1H-indol-2-yl)imidazo[1,2-b]pyridazine (68 mg, 0.141 mmol, 1.0 equiv), xantphos (16 mg, 0.0282 mmol, 0.2 equiv), palladium acetate (3 mg, 0.0141 mmol, 0.1 equiv), and potassium carbonate (389 mg, 2.82 mmol, 20 equiv) in dioxane (5.0 mL) was added 3,4-dimethoxyaniline (24 mg, 0.155 mmol, 1.1 equiv) and heated to 110° C. for 2 h. Purification by column chromatography using 2% methanol in dichloromethane elution gave 20 mg of the yellow solid.

후처리

  1. customPurification by column chromatography
  2. wash2% methanol in dichloromethane elution

출처 및 근거

ORD 기록
ord-8b97bacafc85492499885ac3ffbf702f
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09370515B2

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