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Water → 3-(Benzyloxy)-N-(4-methylthiazol-2-yl)-5-(pyridin-3-yl)pyridin-2-amine dihydrochloride

HRID 1426118
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HRID 1426118 반응식
[ClH:1].[CH2:2]([O:9][C:10]1[C:11]([NH:17][C:18]2[S:19][CH:20]=[C:21]([CH3:23])[N:22]=2)=[N:12][CH:13]=[C:14](Br)[CH:15]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[N:24]1[CH:29]=[CH:28][CH:27]=[C:26](B(O)O)[CH:25]=1.C(=O)([O-])[O-].[Na+].[Na+].O>COCCOC.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[ClH:1].[ClH:1].[CH2:2]([O:9][C:10]1[C:11]([NH:17][C:18]2[S:19][CH:20]=[C:21]([CH3:23])[N:22]=2)=[N:12][CH:13]=[C:14]([C:26]2[CH:25]=[N:24][CH:29]=[CH:28][CH:27]=2)[CH:15]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 27343783-Pyridinylboronic acidHCID 160614653-(benzyloxy)-5-bromo-N-(4-methylthiazol-2-yl)pyridin-2-amine hydrochloride

생성물 1

HCID 866396683-(Benzyloxy)-N-(4-methylthiazol-2-yl)-5-(pyridin-3-yl)pyridin-2-amine dihydrochloride

시약·촉매·용매 2

HCID 178418476
HCID 178418476, 화합물
촉매
HCID 80711,2-Dimethoxyethane용매

실험 절차

3-(Benzyloxy)-5-bromo-N-(4-methylthiazol-2-yl)pyridin-2-amine (prepared according to Example 1; 0.125 g, 0.332 mmol), pyridin-3-ylboronic acid (0.0490 g, 0.399 mmol), bis(triphenylphosphine)palladium(II) chloride (0.00700 g, 0.00997 mmol), and sodium carbonate (0.106 g, 0.997 mmol) were combined in DME (10 mL), and water (5 mL) and heated overnight at 80° C. The reaction mixture was cooled and partitioned between dichloromethane and water. The layers were separated, and the organic layer was dried, filtered, and concentrated. The residue was purified by silica gel chromatography to afford the title compound as the free base. The free base was dissolved in dichloromethane and 2M HCl in ether was added. The mixture was concentrated to afford 3-(benzyloxy)-N-(4-methylthiazol-2-yl)-5-(pyridin-3-yl)pyridin-2-amine dihydrochloride (0.109 g, 87.6% yield). 1H NMR (DMSO-d6) δ 9.27 (m, 1H), 8.81 (d, 1H), 8.75 (d, 1H), 8.48 (d, 1H), 8.08 (m, 1H), 7.97 (m, 1H), 7.66 (d, 2H), 7.43 (m, 2H), 7.37 (m, 1H), 6.82 (s, 1H), 5.45 (s, 2H), 2.31 (s, 3H). Mass spectrum (apci) m/z=375.1 (M+H-2HCl).

후처리

  1. temperatureThe reaction mixture was cooled
  2. custompartitioned between dichloromethane and water
  3. customThe layers were separated
  4. customthe organic layer was dried
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-b25edb966612475084fe8f81df0909bf
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933077B2

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