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Potassium Carbonate → Methyl 4-(6-methoxypyridin-3-yl)-3,5-dimethylbenzoate

HRID 531246
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HRID 531246 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([CH3:21])[C:11]=1B1OC(C)(C)C(C)(C)O1)[C:5]([O:7][CH3:8])=[O:6].Br[C:23]1[CH:24]=[CH:25][C:26]([O:29][CH3:30])=[N:27][CH:28]=1.C(=O)([O-])[O-].[K+].[K+]>[Pd](Cl)Cl.C(P(C(C)(C)C)[C-]1C=CC=C1)(C)(C)C.[C-]1(P(C(C)(C)C)C(C)(C)C)C=CC=C1.[Fe+2].O1CCOCC1>[CH3:30][O:29][C:26]1[N:27]=[CH:28][C:23]([C:11]2[C:10]([CH3:21])=[CH:9][C:4]([C:5]([O:7][CH3:8])=[O:6])=[CH:3][C:2]=2[CH3:1])=[CH:24][CH:25]=1
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참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 27348955-Bromo-2-methoxypyridineHCID 68021937Methyl 3,5-dimethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate

생성물 1

HCID 90009124Methyl 4-(6-methoxypyridin-3-yl)-3,5-dimethylbenzoate

시약·촉매·용매 2

HCID 178454861HCID 178454861, 화합물촉매
HCID 31275
1,4-Dioxane
용매

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온도
80 °C

실험 절차

Methyl 3,5-dimethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (Step A, 2.79 g, 7.20 mmol), 1,1′-bis(di-tert-butylphoshino)ferrocene palladium dichloride (0.391 g, 0.600 mmol) and 5-bromo-2-methoxypyridine (0.776 mL, 6 mmol) were mixed in a reaction flask which was then evacuated and charged with nitrogen three times. Added 1,4-dioxane (30.0 mL) and 3.0M aqueous potassium carbonate (6.00 mL, 18.00 mmol), evacuated and charged with nitrogen (3×), then stirred overnight at 80° C. The reaction was then partitioned between ethyl acetate and water. After a second water wash, the organic was dried over sodium sulfate, filtered and evaporated. The crude was purified by silica gel chromatography, eluting with 10 column volumes of 4% ethyl acetate/hexanes followed by a gradient of 4-10% ethyl acetate/hexanes over 10 column volumes to give the title compound. 1H NMR (CDCl3, 500 MHz) δ7.94 (d, 1H), 67.79 (s, 2H), 67.36 (dd, 1H), 66.84 (d, 1H), 64.00 (s, 3H), 63.93 (s, 3H), 62.09 (s, 6H).

후처리

  1. customwas then evacuated
  2. additioncharged with nitrogen three times
  3. additioncharged with nitrogen (3×)
  4. customThe reaction was then partitioned between ethyl acetate and water
  5. washAfter a second water wash
  6. dry with materialthe organic was dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe crude was purified by silica gel chromatography
  10. washeluting with 10 column volumes of 4% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-6a33b7209045487d9cb1d3b95263d935
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09353101B2

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