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Hydrochloric Acid → HCID 86702432、化合物

HRID 2278453
ノート
印刷プレビュー

反応式

HRID 2278453 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 6

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 10340Sodium Carbonate2 回HCID 46739017(3-Methylpyridin-4-yl)boronic acid hydrochlorideHCID 86702427HCID 86702427、化合物HCID 178479596HCID 178479596、化合物

生成物 1

HCID 86702432
HCID 86702432、化合物
収率 29.9%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒2 回HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒

反応条件

温度
85 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7c0b77eb03a64614810562bbd50f156a
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133178B2

反応ノート

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