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Hydrochloric Acid → HCID 86702432, 화합물

HRID 2278453
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HRID 2278453 반응식
Br[C:2]1[C:3]([C:16]2[CH:20]=[CH:19][O:18][C:17]=2[CH3:21])=[N:4][C:5]([N:8]2[CH2:13][C@H:12]([CH3:14])[O:11][C@H:10]([CH3:15])[CH2:9]2)=[N:6][CH:7]=1.[ClH:22].B(O)O.C(=O)([O-])[O-].[Na+].[Na+].Cl.[CH3:33][C:34]1[CH:35]=[N:36][CH:37]=[CH:38][C:39]=1B(O)O.Cl.CCOCC>O1CCOCC1.O.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>[ClH:22].[CH3:15][C@H:10]1[O:11][C@@H:12]([CH3:14])[CH2:13][N:8]([C:5]2[N:4]=[C:3]([C:16]3[CH:20]=[CH:19][O:18][C:17]=3[CH3:21])[C:2]([C:39]3[CH:38]=[CH:37][N:36]=[CH:35][C:34]=3[CH3:33])=[CH:7][N:6]=2)[CH2:9]1
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참가 물질

10

반응물 6

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 10340Sodium Carbonate2회HCID 46739017(3-Methylpyridin-4-yl)boronic acid hydrochlorideHCID 86702427HCID 86702427, 화합물HCID 178479596HCID 178479596, 화합물

생성물 1

HCID 86702432
HCID 86702432, 화합물
수율 29.9%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매2회HCID 962Water용매2회HCID 312751,4-Dioxane용매

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온도
85 °C

실험 절차

cis-4-[5-Bromo-4-(2-methyl-3-furanyl)-2-pyrimidinyl]-2,6-dimethylmorpholine (100 mg, 0.284 mmol), 3-methyl-4-pyridinyl)boronic acid HCl (54.2 mg, 0.312 mmol), sodium carbonate (75 mg, 0.710 mmol) and tetrakis(triphenylphosphine)palladium(0) (16.40 mg, 0.014 mmol) were added together in 1,4-dioxane (3 mL) and water (0.500 mL) and the resulting mixture was heated at 85° C. under argon for 4 hours. A further amount of (3-methyl-4-pyridinyl)boronic acid HCl (54.2 mg, 0.312 mmol), sodium carbonate (75 mg, 0.710 mmol) and tetrakis (16.40 mg, 0.014 mmol) were added and the resulting mixture was heated at 85° C. under argon for 18 hours. The reaction mixture was allowed to cool to room temperature, diluted with water and extracted with ethyl acetate (×3). The ethyl acetate layers were combined, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by Biotage SP4 column chromatography eluting with a gradient of 0-60% ethyl acetate and iso-hexane. Product containing fractions were combined and evaporated under reduced pressure. The residue was dissolved in methanol (1 ml), treated with 1M HCl in ether (0.1 mL, 0.100 mmol) and evaporated under reduced pressure. The resulting solid was dried under high vacuum at 40° C. for 18 hours to give the title compound (34 mg, 0.085 mmol, 29.9% yield) as a white solid. LC/MS [M+H]+=365; 1H NMR (400 MHz, d4-MeOD): δ 8.68-8.66 (2H, m), 8.33 (1H, s), 7.92-7.90 (1H, d), 7.25-7.24 (1H, d), 5.75-5.74 (1H, d), 4.74-4.70 (2H, m), 3.72-3.64 (2H, m), 2.73-2.67 (2H, m), 2.49 (3H, s), 2.18 (3H, s), 1.25-1.24 (6H, m).

후처리

  1. temperatureto cool to room temperature
  2. extractionextracted with ethyl acetate (×3)
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure
  5. customThe residue was purified by Biotage SP4 column chromatography
  6. washeluting with a gradient of 0-60% ethyl acetate and iso-hexane
  7. additionProduct containing fractions
  8. customevaporated under reduced pressure
  9. dissolutionThe residue was dissolved in methanol (1 ml)
  10. customevaporated under reduced pressure
  11. customThe resulting solid was dried under high vacuum at 40° C. for 18 hours

출처 및 근거

ORD 기록
ord-7c0b77eb03a64614810562bbd50f156a
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133178B2

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