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Dichloromethane → 2'-Methyl-2-oxo-1,2-dihydro-3,4'-bipyridine-6-carboxylic acid, hydrochloride salt

HRID 2364969
ノート
印刷プレビュー

反応式

HRID 2364969 の反応式
C[O:2][C:3]1[N:8]=[C:7]([C:9]([O:11]C)=[O:10])[CH:6]=[CH:5][C:4]=1B1OC(C)(C)C(C)(C)O1.[Cl:22]CCl.Br[C:26]1[CH:27]=[CH:28][C:29]([C:34](OC)=O)=[N:30][C:31]=1OC.CC1(C)C(C)(C)OB(B2OC(C)(C)C(C)(C)O2)O1.C([O-])(=O)C.[K+]>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[ClH:22].[CH3:34][C:29]1[CH:28]=[C:27]([C:4]2[C:3](=[O:2])[NH:8][C:7]([C:9]([OH:11])=[O:10])=[CH:6][CH:5]=2)[CH:26]=[CH:31][N:30]=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

8

反応物 5

HCID 6344DichloromethaneHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 46311222Methyl 5-bromo-6-methoxypicolinateHCID 68380502Methyl 6-methoxy-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)picolinate

生成物 1

HCID 131731315
2'-Methyl-2-oxo-1,2-dihydro-3,4'-bipyridine-6-carboxylic acid, hydrochloride salt

試薬・触媒・溶媒 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

Synthesis of methyl 6-methoxy-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxylate (C31). [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (740 mg, 0.91 mmol) was added in one portion to a degassed mixture of methyl 5-bromo-6-methoxypyridine-2-carboxylate (C30) (7.42 g, 30.2 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi-1,3,2-dioxaborolane (9.19 g, 36.2 mmol) and potassium acetate (8.88 g, 90.5 mmol) in dioxane (150 mL) at room temperature under argon and the reaction was heated at 100° C. for 18 hours. The mixture was cooled to room temperature, filtered through Celite, washed with ethyl acetate (400 mL) and concentrated in vacuo. Silica gel chromatography (Gradient: 15% to 35% ethyl acetate in heptane) afforded the title compound as a colorless oil, which solidified on standing to form a white crystalline solid. Yield: 7.14 g, 24.4 mmol, 81%. LCMS m/z 212.1 (M for boronic acid+1). 1H NMR (400 MHz, CDCl3) δ 1.37 (s, 12H), 3.97 (s, 3H), 4.06 (s, 3H), 7.67 (d, J=7.3 Hz, 1H), 8.09 (d, J=7.3 Hz, 1H). A second crop of material (1.13 g, 13%) was also obtained from the purification; this contained minor impurities by NMR analysis.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered through Celite
  3. washwashed with ethyl acetate (400 mL)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-60fd297cb5ad4734abf11a0ad98a8feb
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697673B2

反応ノート

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