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Chloropyrazine → 8-(5-Pyrazin-2-ylpyridin-2-yl)-1,4-dioxaspiro[4.5]decan-8-ol

HRID 1809938
ノート
印刷プレビュー

反応式

HRID 1809938 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]([C:8]2([OH:18])[CH2:17][CH2:16][C:11]3([O:15][CH2:14][CH2:13][O:12]3)[CH2:10][CH2:9]2)=[N:6][CH:7]=1.C([Mg]Cl)(C)C.C1(P(C2C=CC=CC=2)CCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Cl[C:53]1[CH:58]=[N:57][CH:56]=[CH:55][N:54]=1>C1COCC1.C/C(/[O-])=C/C(C)=O.C/C(/[O-])=C/C(C)=O.[Ni+2]>[N:54]1[CH:55]=[CH:56][N:57]=[CH:58][C:53]=1[C:2]1[CH:3]=[CH:4][C:5]([C:8]2([OH:18])[CH2:17][CH2:16][C:11]3([O:15][CH2:14][CH2:13][O:12]3)[CH2:10][CH2:9]2)=[N:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 73277ChloropyrazineHCID 742671,2-Bis(diphenylphosphino)ethaneHCID 578032528-(5-Bromopyridin-2-yl)-1,4-dioxaspiro[4.5]decan-8-olHCID 178418918HCID 178418918、化合物

生成物 1

HCID 595561548-(5-Pyrazin-2-ylpyridin-2-yl)-1,4-dioxaspiro[4.5]decan-8-ol収率 19.1%

試薬・触媒・溶媒 2

HCID 9834912
Nickel(II) acetylacetonate
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4.5]decan-8-ol (0.50 g, 1.59 mmol) in THF (7.5 mL) was dropwise added isopropyl magnesium chloride (2 M in THF, 1.8 mL) at rt. After stirred for 1 hour, the solution was degassed with N2 three times. To another degassed solution of THF (2.5 mL) at rt was added nickel acetylacetonate (20 mg, 0.080 mmol) and 1,2-bis(diphenylphosphino)-ethane (32 mg, 0.080 mmol) under N2 flush. After stirred for 10 mins, 2-chloropyrazine (0.155 mL, 1.59 mmol) was added in, and the resulting mixture was stirred for 30 minutes. The mixture was then transferred to a freshly prepared solution of the Grignard reagent prepared previously. The mixture was stirred at rt for 18 hours, and was quenched with saturated NH4Cl solution. The aqueous solution was extracted with ethyl acetate, and the combined organic phase was washed with saline solution (2×50 mL), dried over MgSO4, concentrated in vacuo. The residue was chromatographed on SiO2, eluted with hexane/ethyl acetate (1 to 1), and the appropriate fractions were collected to provide 8-(5-pyrazin-2-ylpyridin-2-yl)-1,4-dioxaspiro[4.5]decan-8-ol (95 mg, 19%) as an oil. LCMS: 314.2 (M+H+, 100%).

後処理

  1. customat rt
  2. customthe solution was degassed with N2 three times
  3. customflush
  4. stirringAfter stirred for 10 mins
  5. stirringwas stirred for 30 minutes
  6. customprepared previously
  7. stirringThe mixture was stirred at rt for 18 hours
  8. customwas quenched with saturated NH4Cl solution
  9. extractionThe aqueous solution was extracted with ethyl acetate
  10. washthe combined organic phase was washed with saline solution (2×50 mL)
  11. dry with materialdried over MgSO4
  12. concentrationconcentrated in vacuo
  13. customThe residue was chromatographed on SiO2
  14. washeluted with hexane/ethyl acetate (1 to 1)
  15. customthe appropriate fractions were collected

出典と根拠

ORDレコード
ord-e457b4bb8f9e4fe9aecc3f4d95140735
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08362003B2

反応ノート

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